LITERATURE


- 1009 results found for "lc"
<< Go back to the previous page (Click here to search from the Literature Section)

LC-10AS Pump Recommended Spare Parts List (LC-014)
The following is a list of recommended spare parts for the LC-10AS Pump. This list encompasses those consumable items which are most frequently replaced.
View here (112 KB)

LC-10AD Pump Recommended Spare Parts List (LC-015)
The following is a list of recommended spare parts for the LC-10AD Pump. This list encompasses those consumable items which are most frequently replaced.
View here (134 KB)

Fast LC Analysis of Soft Drinks
This application note details the separation and detection of five beverage compounds with fast LC gradient conditions.
View here (706 KB)

All roads lead to Rome - Fast LC -How
View here (501 KB)

Reducing Analysis Limitations by Using Multiple Detectors with Ultra Fast LC
Reducing Analysis Limitations by Using Multiple Detectors with Ultra Fast LC
View here (944 KB)

PUMPS: Pulse-Free, Unsurpassed in Reliability, Minimal Maintenance, Proven Precision
Shimadzu’s LC-10AS, LC-10AT, and LC-10AD are pulse-free, unsurpassed in reliability, require minimal maintenance, have proven precision and are suitable for your most sensitive applications.
View here (135 KB)

LC-10AT Pump Recommended Spare Parts List
The following is a list of recommended spare parts for the LC-10AT Pump. This list encompasses those consumable items which are most frequently replaced.
View here (135 KB)

LC-10Ai Pump Recommended Spare Parts List
The following is a list of recommended spare parts for the LC-10Ai Pump. This list encompasses those consumable items which are most frequently replaced.
View here (142 KB)

Analysis of Natamycin in Cheese
View here (44 KB)

Analysis of α-Lipoic Acid in Dietary Supplement
View here (130 KB)

Analysis of N-Methylcarbamate Pesticides in Foods
View here (68 KB)

Determination of Cyanidin-3-Glucoside in Black Soybeans
View here (113 KB)

Determination of Quinoxaline-2-Carboxylic Acid in Pork
View here (40 KB)

Analysis of Capsaicinoids in Spices
View here (50 KB)

Analysis of Sudan Dyes in Foods
View here (50 KB)

Analysis of Canthaxanthin and Astaxanthin
View here (38 KB)

Determination of Coenzyme Q10 in Food
View here (36 KB)

Determination of Drugs in Blood Plasma by “Co-Sense for BA” (Part 7)
View here (33 KB)

Analysis of Malachite Green in Cultured Fish
View here (55 KB)

Analysis of Amino Acids in Vinegar
View here (99 KB)

Analysis of Hyaluronic Acid
View here (56 KB)

Analysis of Lycopene and β-Carotene in Tomato
View here (125 KB)

Determination of Benzoyl Peroxide in Foods
View here (63 KB)

Analysis of Tricyclic Antidepressants
View here (37 KB)

Determination of Drugs in Blood Plasma by “Co-Sense for BA” (Part 6)
View here (39 KB)

Analysis of Enrofloxacin in Broiled Eels
View here (50 KB)

Analysis of Glyphosate in Drinking Water by HPLC
View here (38 KB)

Analysis of Diquat in Drinking Water by HPLC
View here (1730 KB)

Analysis of Chlorogenic Acid in Coffee
View here (49 KB)

Determination of Catechins in Tea
View here (52 KB)

Determination of Sucralose in Soft Drinks
View here (32 KB)

Analysis of Pesticides Residues by HPLC
View here (37 KB)

Analysis of Voglibose by Post-column Fluorometric Detection Method
View here (26 KB)

Analysis of Potassium Bromate in Bread
View here (20 KB)

Analysis of Bromate Ions in Drinking Water
View here (45 KB)

Analysis of Animal Drug (2)
View here (35 KB)

Shim-pack HT-ODS ・New High Throughput HPLC Column
View here (23 KB)

Analysis of Sulfurous Acid Ion
View here (23 KB)

Study of Analytical Conditions for Aldehydes in Ambient Air
View here (27 KB)

Analysis of Bisphenol A using High-Performance Liquid Chromatography
View here (29 KB)

Determination of Fumonisins in Corn
View here (25 KB)

Determination of Formaldehyde and Acetaldehyde in Environmental Air
View here (78 KB)

Determination of Microcystins in Blue-green Algae in Lake Water
View here (107 KB)

Analysis of Chlorophyll (a) in Seawater
View here (141 KB)

Advanced Method Development, overnight
View here (1123 KB)

Tested and approved!
View here (176 KB)

Good day, sunshine
View here (138 KB)

Full Automation with Integrated LC
View here (2,190 KB)

LC-8A Consumable Parts List
This file contains descriptions, part numbers and comments.
View here (68 KB)

LC8A Pump Provides Analytical-to-Prep Scale-Up
The LC8A Pump Provides Analytical-to-Prep Scale-Up, is versatile and easy to use, and offers single point control from system controller or CLASS-VP software.
View here (135 KB)

Fractionation by Preparative LC-MS and Fraction Verification byUltra Fast LC-MS
View here (63 KB)

SIL-10A Autosampler Recommended Spare Parts List (LC-016)
The following is a list of recommended spare parts for the SIL-10A Autosampler. This list encompasses those consumable items which are most frequently replaced.
View here (112 KB)

SIL-6B/9A Autosampler Recommended Spare Parts List (LC-017)
The following is a list of recommended spare parts for the SIL-6B/9A Autosampler. This list encompasses those consumable items which are most frequently replaced.
View here (83 KB)

HPLC Detection of Polynuclear Aromatic Hydrocarbons
The polynuclear aromatic hydrocarbons are a ubiquitous class of highly lipophilic, potentially carcinogenic substances consisting of a large number of individual compounds containing aromatic rings.
View here (1,132 KB)

HPLC Application - Simutaneous Analysis of Formic Acid and formaldehyde
Here we report a new and fast procedure for the LC-MS/MS method optimization for clinical drug monitoring.
View here (182804 KB)

High-Speed, High-Resolution Analytical Applications (Part 9) Simultaneous Determination of Tryptophan Metabolites
View here (64 KB)

Analysis of Biofuel (Part 2) Determination of Formic Acid, Acetic Acid, and Propionic Acid in Biodiesel - Diesel Fuel Blend
View here (31 KB)

Application of High-Speed, High-Resolution Analysis (Part 5) Analysis of Artificial Colorings
View here (110 KB)

Application of High-Speed, High-Resolution Analysis (Part 4) Analysis of Cephem Antibiotics
View here (108 KB)

Application of High-Speed, High-Resolution Analysis (Part 3) Analysis of Isothiocyanates and Sinignin
View here (65 KB)

Analysis of Biofuel (Part 1) Determination of Fatty Acid Methyl Esters and Triglycerides in Biodiesel Blended Fuel
View here (30 KB)

High Speed, High Resolution Analytical Applications (Part 2) Analysis of Isoflavones in Soy
View here (81 KB)

High Speed, High Resolution Analytical Applications (Part 1)Introducing Newly-Developed “Shim-pack XR-ODS” Column
View here (50 KB)

Determination of Polyether Antibiotics in Animal Feeds (Part 2) Analysis using Fluorometric Detection
View here (33 KB)

Determination of Polyether Antibiotics in Animal Feeds (Part 1) Analysis by Post-column VIS Photometric Derivatization Method
View here (55 KB)

GPC Cleanup Methods in Pesticides Residue Analysis of Food(Part2)
View here (78 KB)

Analysis of Hexavalent Chromium by Post-column Derivatization Method
View here (62 KB)

Analysis of Impurities in Drugs by Prominence Series UV-VIS Detectors (Part 2)
View here (39 KB)

Analysis of Malachite Green in Cultured Fish (Part 2) Simultaneous Analysis with Leucomalachite Green
View here (303 KB)

Analysis of Impurities in Drugs by Prominence Series UV-VIS Detectors
View here (71 KB)

Analysis of Bromate by Newly Developed Shim-pack IC-Bromate Column
View here (782 KB)

Analysis of Iprodione, Asulam, Thiophanate-methyl, and Siduron in Drinking Water by HPLC
View here (315 KB)

Analysis of ClO2 -, ClO3 -, and ClO2 in Tap Water by Ion Chromatography
View here (1101 KB)

Analysis of NO2-N in Drinking Water by Ion Chromatography
View here (837 KB)

Direct Injection of Blood Plasma for the Determination of Drugs using “Co-Sense for BA” (Part 5)
View here (53 KB)

Direct Injection of Blood Plasma for the Determination of Drugs using “Co-Sense for BA” (Part 4)
View here (66 KB)

Analysis of Anionic Surfactants by HPLC in Accordance with the Revised Water Quality Testing Method
View here (571 KB)

Application of Evaporative Light Scattering Detector ELSD-LT (Part 3) Analysis of Surfactants
View here (34 KB)

New Standard ODS Column “Shim-pack VP-ODS” Supports
View here (50 KB)

LC Separations under 100% Aqueous Conditions using Pathfinder Columns
View here (162 KB)

Napoleon did not die from arsenic poisoning - ADAIS- Automated poison and drug analysis
View here (855 KB)

Benzodiazepine Analysis by UFLC
This application note details the separation and detection of four benzodiazepines with ultra-fast LC (UFLC) conditions.
View here (96 KB)

Analysis of Barbiturates by UFLC
This application note details the separation and detection of seven barbiturates with ultra-fast LC (UFLC) conditions.
View here (111 KB)

Evaluation of the Current Capabilities of Ultra High Pressure LC and High Temperature LC
UHPLC is becoming an increasingly popular technique for sample analysis due to the ability to reduce analysis times or improve resolution. However, the use of ultrahigh pressures can reduce column lifetime and increase the maintenance requirements of the LC system. Another less commonly used technique to reduce analysis times is the use of high-temperature LC. High-temperature LC has the advantage of reducing system pressure by lowering solvent viscosity and may provide the ability to reduce the organic content of the mobile phase. The use of high-temperature LC has been limited by the number of available columns for this technique. A number of applications will be presented up to 19,000 psi and 150 degrees C for the technique.
View here (991067 KB)

LC-10A Series Detectors Recommended Spare Parts List (LC-018)
The following is a list of recommended spare parts for the SPD-10A/V UV/Vis Absorbance Detector and the RF-10A Fluorescence Detector. This list encompasses those consumable items which are most frequently replaced.
View here (83 KB)

Simultaneous Execution of 3 Separations With a Single LC-10A System
The Shimadzu LC-10A System is a versatile HPLC platform that provides ease of automation and flexibility. In response to a request from a customer performing high throughput clinical applications, we were asked to perform three separate analyses with one automated system. To accomplish this task we configured a system with two automated column selection valves, three pumps and an autosampler with cooler.
View here (73 KB)

Separation Of Nucleotides and Xanthines using The LC-10Ai Bioinert HPLC (LC-024)
Recently, the use of bioinert high performance liquid chromatography has increased concomitantly and most likely as a result of research burgeoning in the areas of protein and peptide chemistry. The utility of these systems stems from methodology designed to preserve biological activity and molecular conformation in biological samples.
View here (114 KB)

Reproducible Gradients at Ultra-Low Flow Rates
A growing number of analysts are using techniques such as microbore HPLC and LC-MS which require flow rates anywhere from 10 uL/Min to 200 uL/min. Several factors must be considered when working in this range: appropriate back pressure for reliable pump performance, efficient mixing in a very limited volume, and reduction of dead volume to minimize run time and bandspreading.
View here (113 KB)

Reduced Solvent Consumption and Operational Costs with Existing LC Systems
Although the introduction of ultra-high speed LC is an effective way to conserve solvent, there is a very significant issue as to how this can be achieved with the existing LC systems in use. This report introduces detailed suggestions on how to most effectively reduce solvent consumption with existing LC systems.
View here (998415 KB)

Nexera XR Application - Quantitation by HPLC and Identificaiton by LC/MS for Total Aflatoxins in Food (Japan)
Here, we introduce the standard quality control analysis by EDX of the widely specified magnesium alloy die casting, AZ91D.
View here (1619969 KB)

LCMS-8030 Application - LC/MS/MS Analysis of Vitamin D3 by the Co-Sense for Impurities System (Japan)
Here, we introduce examples of analysis of cesium in tap water and soil using the AA-7000 atomic absorption spectrophotometer.
View here (961152 KB)

Fraction Collection Chromatography Application: Handy Scaled-Up Method using LC-8A
Recently, preparative chromatography has been widely used to purify synthetic reagents and extracts, and for structural analysis. The column volumes required for preparative chromatography, however, range from 10 to 100 times those of conventional LC columns. The absolute injection amounts for preparative chromatography can range from 10(3) to 10(6) times those of conventional LC analysis. This sometimes makes preparative chromatography difficult to directly implement without changing the original analysis conditions. A simple upgrade, using the Shimadzu LC8A, circumvents this implementation difficulty.
View here (347 KB)

LCMS-IT-TOF Application - Development of a New Proteomics Platform for Label-Free Quantitation Methods by LC/MS/MS Combined with a Novel Nano HPLC System (Japan)
Some life science applications, such as proteomics and metabolomics, require LC/MS/MS with very high sensitivity. Nanoflow LC has been developed for such situations. However, nanoflow LC has some difficulties because of its very low flow rate. Precise gradient control is one such difficulty. Thus, retention time reproducibility has been a big problem for nanoflow LC although it is one of the most critical issues for omics studies, especially for label-free quantitative studies. Here, we introduce Prominence nano with the RFC system, a novel flow control system. This nanoflow LC system has great performance for retention time reproducibility in the gradient mode.
View here (1248007 KB)

On-line Comprehensive RP-LC×RP-LC/IT-TOF for the Analysis of Proteome Isoforms
This bottom-up approach relies on both the power of 2D-LC separation techniques, and the sensitivity of MS (ESI-IT-TOF) detection. After separation by RP-LC×RP-LC is performed at the peptide level, both PDA and MS 2D plots are obtained by means of a dedicated software, which further allows qualitative and quantitative data analysis, as well as spectral comparison/subtraction. Tandem MS data obtained by collision-induced dissociation (CID) of the peptides were used for database search for a-casein and dephosphorylated a-casein, with high sequence coverage.
View here (726122 KB)

LCMS-2020 - Reduces Limitations of HPLC Analysis and UFLC Analysis
As explained above, building an LC/MS system that employs an MS as an LC detector can effectively reduce the limitations of LC analysis. In addition to this, reducing those limitations to the greatest extent possible requires an MS that can handle ultra high speed analysis. The new “LCMS-2020” single quadrupole ultra-fast LC/MS, boldly addresses these requirements.
View here (887 KB)

Analysis of Bromate by Post-column Ion Chromatography
View here (2680 KB)

Determination of Alliin in Garlic
View here (23 KB)

Determination of Theanine in Tea
View here (41 KB)

Analysis of Amino Acids in Fermented Food and Drinks
View here (42 KB)

Determination of Water-Soluble Vitamins in “Foods with Nutrient Function Claims”
View here (43 KB)

Analysis of Phenolic Antioxidants in Food
View here (36 KB)

Analysis of Polyether Antibiotics in Animal Feed
View here (24 KB)

Analysis of antidepressants - Pathfinder HPLC column technology
View here (963 KB)

Analysis of antidepressants - Pathfinder HPLC column technology
View here (963 KB)

High-Speed Analysis of Aldehydes and Ketones
View here (283 KB)

High-Speed Analysis of Lycopene
View here (284 KB)

High-Speed Analysis of Furfural
View here (277 KB)

High Speed Analysis of Phenolic Antioxidants
View here (112 KB)

High Speed Analysis of Organic Acids
View here (204 KB)

High Speed Analysis of Sennosides
View here (116 KB)

High Speed Analysis of Glycyrrhetinic Acid
View here (110 KB)

High Speed Analysis of Sulfa Drugs
View here (136 KB)

High Speed Analysis of Hesperidin
View here (147 KB)

High Speed Analysis of Chlorfluazurons
View here (111 KB)

High Speed Analysis of Chlorhexidine
View here (117 KB)

High-Speed Analysis of Ginsenosides
View here (261 KB)

High-Speed Analysis of Cortisone and Cortisol
View here (252 KB)

Prominence UFLC Next Generation High Throughput-HPLC
View here (1387 KB)

Selecting Detectors for Compounds with No Optical Absorbance
View here (1,618 KB)

Prominence nano System and Applications
View here (987 KB)

Determination of Vitamin E in Hand Lotion
Fat soluble Vitamin E (alpha-tocopherol) is an oil found naturally in plants including wheat germ, rice and cotton seeds. In humans, Vitamin e is a potent antioxidant and is also involved in the metabolism of the trace element selenium.
View here (92 KB)

Determination of Tetrabutylammonium Ion in an Antibiotic Sample
Quaternary ammonium salts such as tetrabutylammonium bromide (TBA+Br-) are often encountered in organic chemistry. The reaction of a quaternary ammonium halide with silver oxide yields a quaternary ammonium hydroxide and a silver halide
View here (96 KB)

Automated Calibration Standard Preparation with the SIL-6B/9A
For HPLC analysis, it is often necessary to generate a calibration curve by injecting standards of several known concentrations and computing response factors based upon the linear regression of a plot peak area (or height) vs concentration.
View here (89 KB)

SIL-10AXL Autosampler Recommended Spare Parts List
The following is a list of recommended spare parts for the SIL-10AXL Autosampler. This list encompasses those consumable items which are most frequently replaced.
View here (132 KB)

SIL-10Ai Autosampler Recommended Spare Parts List
The following is a list of recommended spare parts for the SIL-10Ai Autosampler. This list encompasses those consumable items which are most frequently replaced.
View here (145 KB)

Engineering Plastics Components
Engineering plastics include polyamide, polacetal, denatured polyphenylene oxide, polysulfonyl, polycarbonate, and polyester. The recent development of HFIP (hexafluoroisopropanol) has enabled the analysis of this group of engineering plastic compounds at room temperature.
View here (46 KB)

Analysis of Nucleotides Using ODS Column
Analysis of nucelotides is frequently performed using an ODS column in reverse phase distribution mode. Here, application examples demonstrate the analysis of ATP in rat heart tissue and the analysis of nucleotides in tuna meat.
View here (224 KB)

Identification of Proteins by LC-MALDI System
This application note introduces that protein identification by MS/MS ion search using an LCMALDI system which combines a nano-LC system (Prominence nano-AccuSpot-AXIMA® Performance).
View here (4445 KB)

High Speed Analysis of Low Level Estrogens and Their Metabolites from Biological Samples
Introducing a novel multicolumn approach that uses an ultra-high pressure LC system for Cumulative Multicolumn Sequential Chromatography with different column chemistries for the required resolution, significantly reducing analysis time.
View here (1141919 KB)

Prominence Application - High-Speed Analysis of Polymer Additives (2)
This chromatogram shows results of a high-speed analysis of eight water-soluble vitamins.
View here (339818 KB)

HPLC Application - Analysis of Ethyl a-D-Glucoside in Sake
Here we introduce an example of analysis of gingkolic acids contained in ginkgo biloba leaves.
View here (228956 KB)

HPLC Application - Analysis of Ginkgolic Acids in Ginkgo Biloba Extract
Here we introduce examples of HPLC analysis of 3 active ingredients (chlorhexidine, benzethonium, and benzalkonium) found in commercially available disinfectants.
View here (427911 KB)

HPLC Application - Analysis of Flavonoids in Ginkgo Biloba Extract
Here, we introduce an example of analysis of the hexafluorophosphate ion in electrolytic solution used in lithium-ion rechargeable batteries by UHPLC.
View here (1190331 KB)

Nexera Application - Use of Methanol Solvent for Separation
Here we introduce an example of analysis of methyl methacrylate in plastics in which polymethyl methacrylate is the main ingredient.
View here (163039 KB)

Analysis of Halogens in Polyphenylene Sulfide Resin Using a Combustion-Ion Chromatography System
Here we introduce an example of analysis of halogen in a commercially available polyphenylene sulfide (PPS) resin using a combustion-ion chromatography system.
View here (1517689 KB)

HPLC Application - High Speed Analysis of Catechins
The chromatogram is an example of a high-speed analysis of catechins. A UV detector was used for the detection of catechins. For LCMS detection, please refer to Data Sheet No. 26.
View here (270262 KB)

Analysis of Melamine and Its Related Substances in Fertilizers
This article introduces an example of the analysis of melamine and related substances in fertilizers using an HPLC system, with reference to the fertilizer test methods (2012) under the supervision of the Japan‘s Food and Agricultural Materials Inspection Center (FAMIC).
View here (191975 KB)

HPLC Application - Analysis of Mannitol Using RID-20A Differential Index Detector
This Application Datasheet introduces measurements of phthalate ester standard samples using the PyScreener.
View here (867514 KB)

Nexera-e Application - On-line Comprehensive RP-LCxRP-LC/IT-TOF for the Analysis of Proteome Isoforms (Japan)
Polyphenols in sugarcane (Saccharum spp.) leaf extracts were analyzed by comprehensive two-dimensional liquid chromatography in combination with photodiode array and mass spectrometry (LC×LC-PDA-MS) detection; a micro cyano and a partially porous octadecylsilane column were employed in the first and the second dimension, respectively. Even using RP mode in both dimensions, a satisfactory degree of orthogonality was achieved by employment of different approaches of gradient elution mode in the second dimension. By means of the investigated set-up, a total of 38 polyphenolic compounds were detected with the complementary data of PDA, MS and an in-house database.
View here (1545870 KB)

Separation of Tryptic Digest of Cytochrome C Using LC-7A Liquid Chromatograph
The chromatographic analysis of the tryptic digest of cytochrome C, along with many biological separations, pose special problems for standard HPLC systems. Typically mobile phases containing high salt concentrations (e.g. 1 M NaCl), or other corrosive agents such as trifluoroacetic acid, are used which will degrade the stainless steel in HPLC pumps unless the system is carefully passivated and rigorously maintained.
View here (83 KB)

The Analysis of Analgesics by UV Detection
In the pharmaceutical industry, different chromatographic techniques are used in method development and drug analysis. HPLC is the most common analytical technique used in the analysis of many compounds including Analgesics, Antiarrhythmics, Antibacterials, Cardiac drugs, Cholesterol-Reducing drugs, and Vitamins. The Shimadzu LC-10A Series HPLC System provides the sensitivity, reliability and precision required for pharmaceutical analyses
View here (103 KB)

SIL-10AXL Autosampler Semi-Micro Kit (LC-031)
The utility and demand for semi microbore HPLC has dramatically increased for a variety of reasons: semi-microbore applications offer increased sensitivity, reduced sample consumption and a substantial reduction in liquid waste. Shimadzu now offers the option of implementing a semi-micro kit to easily and economically convert the SIL-10AXL analytical autosampler to an autosampler capable of semi microbore applications.
View here (141 KB)

Analysis of Additives in Polymers Using Fraction Collection LC-FTIR
Infrared spectroscopy is an excellent method for identification of compounds. However, when the absorbance of components overlap, it is more difficult to identify each component. In this type of situation, it is more necessary to combine this method with a separation method such as gas chromatography (GC) or liquid chromatography (LC).
View here (125 KB)

Evaluation of Kinetex Column Peak Capacity Using the Shimadzu Nexera UHPLC System
Peak capacities of 200 could be obtained with a 24 second gradient runtime for the compounds that were tested. All compounds were eluted from the column in less than 15 seconds. These results demonstrate the combined benefits of high column efficiency and system performance.
View here (384635 KB)

High Speed, High Resolution Analysis (Part 34) Analysis of Preservatives in Cosmetics by the Nexera UHPLC System
High-speed analysis of preservatives in cosmetics was previously introduced in Application News No. L375, but we have updated this application as an example of ultra-high-speed analysis with the Nexera LC system in conjunction with the Shim-pack XR-ODS III high-speed separation column (particle size 1.6 μm).
View here (1356736 KB)

High Speed, High Resolution Analysis (Part 36) Analysis of Quinolones by the Nexera UHPLC System
Many types of quinolone synthetic antibacterials are widely used for the prevention and treatment of infectious diseases in domestic animals, domestic fowl, and cultured fish. Here, we introduce an example of simultaneous analysis of a mixture of synthetic quinolone antibacterials using the Nexera ultra high performance LC system with the RF-20Axs high-sensitivity fluorescence detector.
View here (1342828 KB)

LCMS-8050 Application - Glycerophospholipids Analysis by Comprehensive HPLC Coupled with a Triple Quarupole Mass Spectrometer (Japan)
This work demonstrates the exibility and utility of a completely online, automated solution for LC-MS/MS sample preparation and peptide analysis using both data dependent and targeted work flows.
View here (1009444 KB)

LCMS-8040 Application - A Fast LC/MS/MS method for Determination of Telmisartan in Human Plasma by LC-MS-MS (Asia Pacific)
A fast LC/MS/MS method for quantitative determination of Telmisartan in human plasma using UHPLC Nexera coupled to LCMS-8040 Triple Quadrupole Mass Spectrometer was described. A simple protein precipitation method for extraction of Telmisartan with internal standard (Irbesartan) from the biological matrix was employed. The new advanced LCMS-8040 enabled the quantification of Telmisartan from human plasma samples over a concentration range of 4.0 (LLOQ) to 2000 ng/mL. The constructed calibration curve was linear with a regression of coefficient more than 0.99.
View here (237636 KB)

LCMS-IT-TOF Application - On-Line Comprehensive RP-LCxRP-LC/IT-TOF for the Analysis of Proteome Isoforms
This bottom-up approach relies on both the power of 2D-LC separation techniques, and the sensitivity of MS (ESI-IT-TOF) detection. After separation by RP-LC×RP-LC is performed at the peptide level, both PDA and MS 2D plots are obtained by means of a dedicated software, which further allows qualitative and quantitative data analysis, as well as spectral comparison/subtraction. Tandem MS data obtained by collision-induced dissociation (CID) of the peptides were used for database search for α-casein and dephosphorylated α-casein, with high sequence coverage.
View here (518732 KB)

Integration of Amino Acid, Acylcarnitine and Steroids Analysis in Single FIA/LC-MS/MS Platform
Analysis of amino acids (AA) and acylcarnitines (AC) in dried blood spot (DBS) sample collection method by #31;flow injection analysis (FIA) is now widely used. On the other hand, traditionally, analysis of steroid such as 17-hydroxyprogesterone is done by immunoassays but LC/MS/MS will be an attractive analytical alternative because it can also screen for other related steroids. The use of LC/MS/MS results in a reduction of false positives and a more accurate quantitative performance. The requirements against steroid analysis by LC/MS/MS are getting more stringent issues. In this study, we present a strategy for performing both AA/AC and steroids analysis within a single LC/MS/MS platform.
View here (998564 KB)

LCMS-2020 Application - Stop-flow Comprehensive Two-dimensional Liquid Chromatography Combined with Mass Spectrometric Detection for Phospholipid Analysis
A novel comprehensive two-dimensional liquid chromatographic (LC×LC) system for characterization of phospholipid (PL) molecular species belonging to six phospholipid classes was developed. To tackle such a task, a silica hydrophilic interaction liquid chromatography (HILIC) column was used as the rst dimension (D1), and reversed-phase liquid chromatography (RP-LC) with a C18 column was used as the second dimension (D2) in combination with mass spectrometric detection. Fraction transfer from the D1 to the D2 was performed by means of a two-position ten-port switching valve, operated under stop-ow conditions. The capability of the investigated LC×LC approach was demonstrated in the separation of phospholipid molecular species contained in two Folch-extracted cow’s milk and plasma samples.
View here (324154 KB)

LCMS-8050 Application - High Throughput Quantitation for Therapeutic Drug Monitoring with Open Access LC/MS/MS System (MSACL)
In this paper, we introduce four research use only LC/MS/MS methods for therapeutic drug monitoring (TDM), mycophenolic acid, sunitinib and axitinib, voriconazole, itraconazole. TDM is indispensable for managing drug dosage based on the drug concentration in blood in order to conduct a rational and efficient drug therapy. Liquid chromatography coupled with tandem quadrupole mass spectrometry (LC/MS/MS) is increasingly used in TDM because it can perform selective and sensitive analysis by simple sample pretreatment. In the field of TDM, it is necessary to measure the specimen such as plasma or serum quickly after suitable pretreatment and report the precise result. LC/MS/MS system with a simple and user-friendly interface can provide a streamlined workflow and reduce the load of analysts. We developed high-throughput LC/MS/MS methods for TDM with a new data acquisition and processing software.
View here (1055210 KB)

Guaranteed Scale-Up From Analytical to Preparative with Shimadzu Matched Column Sets
Development of an HPLC can be a time consuming process. Development of a preparative HPLC method can be expensive as well as time consuming, when the cost of the solvents being pumped at preparative flow rates is taken into consideration. Shimadzu provides a solution to this problem by offering matched column sets with the scale-up from analytical to preparative guaranteed.
View here (85 KB)

Fraction Collection - B Carotene in Carrot Extract
b-carotene is contained in carrots, pumpkins, tomatoes, and other produce. It is an essential vitamin A precursor. An HPLC recycling valve separation technique was developed for the analysis of b-carotene from carrot extract. The effect of the recycling method was then confirmed using a photodiode array detector.
View here (94 KB)

Determination of Stavudine Utilizing Semi-Microbore Electrospray LC/MS
It is generally accepted that sensitivity of electrospray ionization LC/MS (ESI) isconcentration dependant, i.e., overall method sensitivity can be enhanced by scaling down the column diameter,flow rate and amount of sample injected on-column.
View here (153 KB)

LCMS-8030/8040 Application - Analysis of Serotonin using LC-MS-MS (SSI)
Perfluorocarbons (PFCs) and their derivatives have many industrial uses but pose environmental and health concerns. Sensitive and selective methods for detection of perfluorocarbons by LC-MS-MS are needed.
View here (267631 KB)

Measuring Samples Per USP <643> Using Shimadzu TOC-LC*H
Shimadzu’s TOC-LC*H analyzer is perfectly adapted to meet the requirements of USP Method <643>. The TOC-LC*H analyzer utilizes 680°C heat and platinum catalyst to provide a lower maintenance instrument with a detection limit of 0.0040 mg per liter.
View here (398438 KB)

LCMS-8050 Application - Biomonitoring Platform for Measuring Pesticide Levels in Tissue - Capillary LC/MS Analysis of Pesticides in Plasma from Noviplex Cards (SSI)
This study presents a custom LC-MS system that allows separaIon and chromatographic development and quanItaIve determinaIon of proteins and small molecules in the same sample using triple quadruple mass spectrometer.
View here (9311342 KB)

LCMS-8050 Application - Highly Sensitive and Rapid Simultaneous Method for 45 Mycotoxins in Baby Food Samples by HPLC-LC/MS Using Fast Polarity Switching (Europe)
In this preliminary evaluation, warfarin concentration was measured by LC/MS/MS to evaluate if PSC technology could complement INR when sampling patient blood.
View here (239389 KB)

LCMS-8040 Application - Quantitative Proteomics of Metabolic Enzymes in S. cerevisiae Using Triple Quadrupole LC/MS/MS (Japan)
The integrated LC system Nexera-i (LC-2040) coupled to the LCMS-8050 triple quadrupole mass spectrometer was tested for chromatographic performance and reproducibility.
View here (778519 KB)

Increase Your Productivity with our State-of-the-Art Autosamplers
Increase Your Productivity with our State of the Art Autosamplers
View here (212 KB)

Application of HPLC to the Analysis of Cosmetics
For the analysis of antiseptics and disinfectants contained in cosmetics, applicable methods of analysis are GC, UV-Vs spectrophotometry and HPLC.
View here (428 KB)

Analysis of Ointment
By using HPLC, active ingredients in products can be identified and determined in a short time, only by a very simple pretreatment.
View here (50 KB)

Applications of HPLC to Pharmacognosy
Active ingredients in crude drugs vary in contents depending on the sampling time and place of origin, and the qualty evaluation of the crude drugs is determined by the contents of the ingredients.
View here (70 KB)

Applications in Food Analysis (16)
The fungicide methods shown here, to protect plants and fruit, were adopted from the reversed phase ion-pair chromatographic technique for these substances
View here (54 KB)

Application of Preparative Liquid Chromatography (3)
In order to successfully conduct a recycle separation, it is necessary to reduce extra-column band broadening.
View here (62 KB)

Analysis of Cyanide Ion and Cyanogen Chloride by Post-column Ion Chromatography
View here (138 KB)

Application of Evaporative Light Scattering Detector ELSD-LT (Part 2) Analysis of Oligosaccharides in Beer
View here (71 KB)

Direct Injection of Blood Plasma for the Determination of Drugs using “Co-Sense for BA” (Part3)
View here (35 KB)

Application of Evaporative Light-Scattering Detector “ELSD-LT”(Part1) Analysis of Triglycerides in Cooking Oil
View here (39 KB)

Determination of Hydrocarbon Types in Diesel Fuel According to the JPI* Method *(Japan Petroleum Institute)
View here (53 KB)

Direct Injection of Blood Plasma for the Determination of Drugs using “Co-Sense for BA” (Part 2)
View here (52 KB)

Direct Injection of Blood Plasma for the Determination of Drugs using “Co-Sense for BA” (Part 1)
View here (62 KB)

HPLC Analysis of Isocyanuric Acid and LAS Anionic Surfactant by the JWWA* Method (* Japan Water Works Association)
View here (53 KB)

HPLC Analysis of Carbofuran, Methomyl, and Carbaryl by the JWWA* Method (* Japan Water Works Association)
View here (28 KB)

Rapid and Sensitive Analysis of Aluminum Ions using On-column Derivatization (Part 1)
View here (22 KB)

AXIMA-TOF2 LC-MALDI Software Guide
View here (278 KB)

AXIMA-TOF 2-Protein Identification of Complex Mixtures using LC-MALDI on AXIMA-TOF2
View here (216 KB)

AXIMA-QIT - Characterization of Complex Protein Gel Bands by Offline LC-MALDI QIT TOF MS
View here (110 KB)

Analysis of Analgesics by UFLC
This application note focuses on the high-speed analysis of over-the-counter analgesics with Ultra Fast HPLC.
View here (159 KB)

High-Speed Analysis of Pesticides in Water Quality Regulation
View here (284 KB)

High-Speed Analysis of Fat-Soluble Vitamins
View here (282 KB)

High Speed Analysis of Vitamin D
View here (140 KB)

High Speed Analysis of Sudan Dyes
View here (131 KB)

High Speed Analysis of Polynuclear Aromatic Hydrocarbons (PDA Detection)
View here (138 KB)

High Speed Analysis of Synthetic Sweeteners
View here (136 KB)

High Speed Analysis of Vitamin B12
View here (134 KB)

High Speed Analysis of Amino Acids by Pre-Column Derivatization (2)
View here (140 KB)

High Speed Analysis of Amino Acids by Pre-Column Derivatization (1)
View here (141 KB)

High Speed Analysis of Food Preservatives
View here (142 KB)

High Speed Analysis of &alpha;-Lipoic Acid
View here (156 KB)

High Speed Analysis of Scopolamine and Hyoscyamine
View here (109 KB)

High Speed Analysis of Coenzyme Q10
View here (114 KB)

High-Speed Analysis of Malachite Green and Metabolites
View here (253 KB)

Principles and practical applications of Shimadzu's ELSD-LTII evaporative light scattering detector
View here (1593 KB)

Migration points to fast analysis; Optimization of the system and analysis conditions
View here (2783 KB)

Applications of Ultra Fast HPLC
This application note focuses on the high-speed analysis of xanthine derivatives and triarylmethane ink dyes with Ultra Fast HPLC.
View here (175 KB)

Analysis of Water Treatment Samples
Analysis of Water Treatment Samples with Shodex Columns.
View here (147738 KB)

Analysis of Water Treatment Samples - Ammonium
Analysis of Water Treatment Samples with Ammonium using Shodex Columns.
View here (143652 KB)

Determination of Chlorhexidine, Benzethonium, and Benzalkonium in Disinfectants
Here we introduce examples of HPLC analysis of 3 active ingredients (chlorhexidine, benzethonium, and benzalkonium) found in commercially available disinfectants.
View here (233115 KB)

Analysis of Electrolytic Solvents for Lithium-Ion Rechargeable Battery
In this application news we introduce an example of analysis of electrolytic solvents used in lithium-ion rechargeable batteries by HPLC.
View here (954089 KB)

Analysis of Steviol Glycosides in Stevia Extract
We introduce an example of analysis of the 9 major steviol glycosides in the stevia extract by reversed phase chromatography.
View here (935491 KB)

LCMS-8050 Application - Integration of Amino Acid, Acylcarnitine and Steroids Analysis in Single FIA/LC-MS/MS Platform (Japan)
Analysis of amino acids (AA) and acylcarnitines (AC) in dried blood spot (DBS) sample collection method by flow injection analysis (FIA) is now widely used. On the other hand, traditionally, analysis of steroid such as 17-hydroxyprogesterone is done by immunoassays but LC/MS/MS will be an attractive analytical alternative because it can also screen for other related steroids. The use of LC/MS/MS results in a reduction of false positives and a more accurate quantitative performance. The requirements against steroid analysis by LC/MS/MS are getting more stringent issues. In this study, we present a strategy for performing both AA/AC and steroids analysis within a single LC/MS/MS platform.
View here (1021317 KB)

Dual Wavelength Detection of a Peptide
When it comes to demanding HPLC applications, you need a reliable system providing the ultimate in flexibility and performance. The Shimadzu LC-10A Series is such a system. While every analysis is not as difficult to perform as trifluoroacetic acid (TFA)/acetonitrile peptide separations, wouldn't it be nice to have equipment which is equal to the task, reliable enough for routine applications and also a good value? Of course it would! That's why you need to look no further than Shimadzu's LC-10A.
View here (101 KB)

Determination of Serum Extracts Plus Reserpine Spikes Utilizing SPE and ESI on QP-8000
This application note describes the determination of reserpine in serumutilizing the Solid Phase Extraction (SPE) and electrospray (ESI) in LC/MS.
View here (172 KB)

On-Column Detection Limit for Testosterone by APLC LC/MS
Atmospheric pressure chemical ionization (APCI) LC/MS offers users a highly-sensitive and specific means for the determination of non-polar and semi-polar analytes, including steroids such as testosterone
View here (71 KB)

Fraction Collection Options with Discovery VP
The Discovery VP preparative system is designed for purification of compounds generated by reaction processes such as combinatorial chemistry and multi-step organic synthesis, or for isolation of analytes in naturally occurring substances.
View here (63 KB)

Achieving Ultra-High-Speed Analysis with LC/MS/MS
This report addresses the problems associated with conventional LC/MS/MS systems in achieving ultra-high-speed analysis, and introduces a resolution to these problems.
View here (711901 KB)

LCMS-8030/8040 Application - Oil Dispersants (SSI)
An extremely fast LC-MS-MS method for the determination of mycotoxins and other untargeted chemical threats was developed.
View here (262883 KB)

LCMS-8040 Application - Characterization of Flavonoids and Phytoestrogens in an Extract of Pueraria Mirifica by UHPLC-MS-MS (SSI)
Inspection results for 138 pesticides using GC/MS/MS and LC/MS/MS have been reported by the EURL (European Union Reference Laboratory). Of the 138 substances, it was recommended that 66 of those substances be analyzed using the triple quadrupole GC/MS/MS, and that the remaining 72 substances be analyzed by the triple quadrupole LC/MS/MS. Thus, the pesticides were analyzed using the GCMSTQ8030 and LCMS-8040 as recommended. The combined use of GC/MS/MS and LC/MS/MS permits high-sensitivity comprehensive analysis of residual pesticides in foods.
View here (217673 KB)

LC/MS/MS Analysis of Impurities in Active Pharmaceutical Ingredients Using the Co-Sense for Impurities System
Detection of impurities in active pharmaceutical ingredients (APIs) is often conducted using an HPLC-UV method. However, qualitative and quantitative analysis of impurities requires not only the separation of the impurities from the major component, but also separation among impurities themselves. The time and effort required to establish effective analytical conditions for this type of analysis are significant. Furthermore, the source of the impurity, whether it be the sample itself or some external factor associated with a particular lot, must also be determined. Here we demonstrate analysis of an impurity in an API using the 2-dimensional LC/MS/MS separation feature of the Co-Sense for Impurities System.
View here (1335216 KB)

Analysis of Compounds Containing a Phosphate Group Using the New MastroTM High Pressure-Resistance Stainless Steel- Free LC Column
Here, we examined the effects of different flow line materials on the peak shape of coordination compounds. Also, using a formic acid mobile phase, which is commonly used in LC/MS analysis, we examined the inhibiting effect on metal adsorption of coordination compounds that is provided with MastroTM high pressure-resistance stainless steel-free analytical column.
View here (1217000 KB)

LCMS-8050 Application - Development of 2D-LC/MS/MS Method for Quantitative Analysis of 1a,25-dihyroxylvitamin D3 in Human Serum (Asia Pacific)
This study demonstrates a platform for biomonitoring levels of these compounds harnessing the simplicity of collecting small blood droplets coupled to the versatility and sensitivity of capillary LC-MS quantitation.
View here (309810 KB)

HPLC Application - Simultaneous Analysis of Water Soluble Vitamins by Newly Developed Shim-Pack MAqC ODS I Column
Here, it is demonstrated that LC/MS measurement using the Shim-pack MAqC-ODS I is indeed possible by desalting using an automated pretreatment system such as the Co-Sense for LC/MS. Analysis of famotidine is also introduced as an example of analysis of impurity in pharmaceuticals using the Shim-pack MAqC-ODS I.
View here (1025474 KB)

LCMS-8050 and IT-TOF Applicaiton - A Comparative Study of Targeted Screening Method by LC/MS/MS and Un-Targeted Screening Method by LC-TOF in Residual Pesticides Analysis (Asia Pacific)
Advanced screening methods based on liquid chromatography-mass spectrometry (LC-MS) for detection of un-predicted residues of pesticides and veterinary drugs in agriculture products and food have been reported in recent years. Without spectrum libraries like in GCMS, LC/MS/MS was initially not used in screening analysis. Whereas, high resolution LC-TOF was selected for screening analysis due to its accurate mass capability. However, with rapid progress in data acquisition technique speed like UFMS (ultrafast MS) and high MRM capacity, new generation triple quadrupole LC/MS/MS has been used for targeted screening, e.g., of over a few hundred of pesticides in one analysis. It is interesting to know the advantages and limitations of the two different screening approaches for pesticide residues in agriculture and food matrixes. We describe here a comparative study on targeted screening analysis based on MRM method on a UFMS-TQ system and un-targeted screening analysis based on high resolution MS full spectrum method on a LC-TOF system using same sample sets of mixed pesticides aiming at unveiling their capabilities and limitations in the challenging screening analysis.
View here (836083 KB)

Analysis of Haloacetic Acids in Drinking Water Using Triple Quadrupole LC/MS/MS (LCMS-8050)
This Application News introduces the use of the LCMS-8050 triple quadrupole mass spectrometer for analysis of these HAAs in accordance with the official LC/MS methodology requirements.
View here (841545 KB)

Analysis of Phenols in Drinking Water Using Triple Quadrupole LC/MS/MS (LCMS-8040)
Here, we introduce an example of phenol analysis by UHPLC/MS/MS. Unlike the use of GC/MS for this analysis, LC/MS/MS does not require derivatization, and therefore simplifies the analysis process
View here (883542 KB)

Analysis of Nivalenol, Deoxynivalenol, 3-Acetyldeoxynivalenol and 15-Acetyldeoxynivalenol Using Triple Quadrupole LC/MS/MS (LCMS-8050)
This paper describes an LC-MS/MS method for highsensitivity simultaneous analysis of the four compounds, nivalenol, deoxynivalenol and the deoxynivalenol metabolytes, 3-acetyl-deoxynivalenol and 15-acetyldeoxynivalenol.
View here (956546 KB)

Analysis of Diarrhetic Shellfish Toxin Using Triple Quadrupole LC/MS/MS (LCMS-8050)
Analysis of Diarrhetic Shellfish Toxin Using Triple Quadrupole LC/MS/MS (LCMS-8050)
View here (955526 KB)

Evaluation of MS Scanning Speeds with UHPLC Peak Widths
The trend toward high-speed LC analysis with reduced column particle sizes continues to increase in popularity. The narrow peak widths of high-speed LC have generally been handled adequately with UV detectors by increasing data acquisition rates. However, use of a MS will reduce the risk of misidentifying peaks when transferring methods from conventional to high-speed LC. Most MS instruments have had difficulty keeping up with these sharp peaks, which may have peak widths of 200 milliseconds or less. Accurate mass analysis of sharp chromatographic peaks obtained by high-speed LC requires ultra-fast MS detection capabilities. A number of high-speed separations will be evaluated using MS scanning speeds of up to 15,000 u/sec with polarity switching speeds of 15 msec.
View here (1100389 KB)

Nexera Application - High Speed, High Resolution Analysis (Part 46) Analysis of Pre-Column Derivatized Biogenic Amines by the Nexera SIL-30AC Autosampler
Scientists rely on LC-MS-MS for detection and quantitation of nucleosides. LC-MS-MS methods use MRM analysis for the highest sensitivity and selectivity; however these methods only detect analytes whose MRM transitions are known in advance. Modified nucleosides are not easily identified by traditional MRM-based methods as many species share common precursor and product ions. Product ion scanning, in conjunction with chromatographic separation, may be used to identify them. We developed LC-MS methods that utilize extremely fast product ion scanning for detection of nucleosides obtained from commercial suppliers. Product ion spectra for each known nucleoside were acquired and inspected for common product ions. A mixture of modified nucleoside standards was analyzed as well.
View here (1149693 KB)

LCMS-8050 Application - Analysis of Polysorbates in Biotherapeutic Products using Two-Dimensional HPLC Coupled with Mass Spectrometer (SSI)
In order to detect many kinds of amino acids with high selectivity in food samples, the LC/MS analysis have been used widely. Amino acids are high polar compound, so they are hard to be retained to reverse-phased column such as ODS (typical method in LC/MS analysis). It needs their derivartization or addition of ion pair reagent in mobile phase to retain them. For easier analysis of amino acids, it is expected to develop the method without using reagents mentioned above. This time, we tried to develop a simultaneous high sensitive analysis method of 20 amino acids by LC/MS/MS with mix-mode column (ion exchange, normal-phase) and the typical volatile mobile phase suitable for LC/MS analysis.
View here (219932 KB)

i-Series Application - Analysis of Quasi-Drug by Nexera-i (Part 1) High-Speed, High-Resolution Analysis of Active Ingredient and Preservatives
Here, using the new Prominence-I integrated high-performance liquid chromatograph, we conducted analysis of substances chemically related to bepotastine besilate in accordance with the Japanese Pharmacopoeia, while at the same time comparing the analysis results between those using the Prominence-I (with the standard configuration or with the delay volume-compatible system kit) and those obtained using both the conventional integrated LC-2010 model as well as a third-party company’s LC system. In addition, we introduce an example of method transfer from that used with Shimadzu’s conventional system or that of a third-party LC system, respectively. At the same time, we introduce an example of high-speed analysis using the Prominence-I (with Low-volume tubing kit installed) in which the analysis time is shortened to about one-fourth the time, while conforming to the Japanese Pharmacopoeia default of conditions.
View here (971216 KB)

Nexera-e Application - Comprehensive LC X LC Analysis of Flavoring Ingredients in Distilled Spirits (SEG)
Composition of flavoring ingredients in distilled spirits is largely dependent on make and storage of the product after distillation. The so-called “aging” of alcoholic beverages takes place in charred wooden, mostly oak barrels. During this process of maturation, wood components are extracted into the distillate, which has a major effect on their final aroma. The complex composition and a distinct change over the period of storage in the cask provide a unique profile for any distilled spirit after “aging”. Due to anaerobic decomposition of the lignin underneath the wood charcoal layer in the cask, aromatic aldehydes, such as vanillin or p-anisaldehyde are formed. Colour and (poly-)phenol content of the distillate are a result of extractable wood components. Additional flavoring ingredients are formed by oxidative, interactive chemical reactions of the various constituents.
View here (971666 KB)

Simultaneous Analysis of Irganox Polymer Additive using LC-MS
View here (178 KB)

Analysis of Phenoxyproprionic Type Herbicides using LC-MS
View here (168 KB)

Analysis of Bisphenol A Diglycidyl Ether Using LC-MS
View here (153 KB)

Analysis of Microcystins Using LC-MS
View here (192 KB)

Drug analysis using Co-Sense for BA LC-MS system (1)
View here (128 KB)

Analysis of fullerenes using LC-MS
View here (126 KB)

Analysis of alkyl phenyl polyoxyethylene sulfonate using LC-MS
View here (160 KB)

Analysis of benzalkonium and polyoxyethylene lauryl ether using LC-MS
View here (126 KB)

Analysis of fatty acid amidopropylbetaine using LC-MS
View here (128 KB)

Analysis of pesticides in foods using LC-MS
View here (145 KB)

Analysis of alkylphenols using LC-MS
View here (390 KB)

Analysis of Vitamin K in food using LC-MS
View here (135 KB)

Analysis of penicillin analogue using LC-MS
View here (152 KB)

Analysis of Bisphenol A and Nonylphenol using LC-MS
View here (155 KB)

Analysis of DNPH-aldehydes using LC-MS
View here (158 KB)

Analysis of antioxidants in drug and food using LC-MS
View here (233 KB)

Analysis of Proteins and Peptides using LC-MS
View here (217 KB)

Analysis of Sudan Dyes and Para Red using LC-MS
View here (73 KB)

Analysis of Steroidal Anti-Inflammatory Drugs Using LC/MS
View here (64 KB)

Drug Analysis Using “Co-Sense for BA” LC/MS System (2)
View here (62 KB)

LC-MSAnalysis of Compounds Related to Nucleic Acids
View here (64 KB)

Simultaneous Analysis of Pesticides in Environment Water using LC-MS
View here (166 KB)

Simultaneous Analysis of Pesticides using LC-MS
View here (78 KB)

Simultaneous Analysis of Carbamate Pesticides with LC-MS
View here (183 KB)

Analysis of N-nitroso-fenfluramine using LC-MS
View here (51 KB)

Application using Analytical / Preparative LC-MS System (Part 1)
View here (316 KB)

Analysis of Perfluorochemicals (PFOA, PFOS) using LC-MS
View here (48 KB)

High-Speed Analysis of Glycyrrhizinate
View here (279 KB)

High-Speed Analysis of Berberine
View here (280 KB)

High-Speed Analysis of Catechins
View here (288 KB)

High-Speed Analysis of Curcumin
View here (281 KB)

TOC Application - TOC-L - Measuring Samples per USP <643> Using Shimadzu TOC-LC*H - Long Version
The United States Pharmacopoeia has established guidelines for determining system suitability and established the acceptance of Water For Injection (WFI) purposes and Purified Water (PW) (USP Method <643>). Shimadzu’s TOC-LC*H analyzer is perfectly adapted to meet the requirements of USP Method <643>. The TOC-LC*H analyzer utilizes 680°C heat and platinum catalyst to provide a lower maintenance instrument with a detection limit of 0.0040 mg per liter.
View here (557045 KB)

LCMS-8040 Application - Analysis of Linear Alkylbenzene Sulfonate in Environmental Water Using Online SPE LC System Coupled with LC-MS/MS (Japan)
Optimization of peak separation and sensitivity is important for decision of LC/MS analytical conditions. However, the evaluation of them has been tedious and time-consuming operation. The HPLC method scouting system coupled to single quadrupole mass spectrometer used in this study can dramatically shorten total run time compared with the conventional system, because this system can make enormous combinatorial analysis methods and run batch program automatically. In this study, we developed the optimized method for the simultaneous analysis of seventeen kinds of sugars based on the result of evaluation for columns, mobile phases and gradient programs using this system.
View here (165548 KB)

Analysis of Pesticides in Food Matrix using QuEChERS by Triple Quadrupole GC/MS/MS and LC/MS/MS
Inspection results for 138 pesticides using GC/MS/MS and LC/MS/MS have been reported by the EURL (European Union Reference Laboratory). Of the 138 substances, it was recommended that 66 of those substances be analyzed using the triple quadrupole GC/MS/MS, and that the remaining 72 substances be analyzed by the triple quadrupole LC/MS/MS. Thus, the pesticides were analyzed using the GCMSTQ8030 and LCMS-8040 as recommended. The combined use of GC/MS/MS and LC/MS/MS permits high-sensitivity comprehensive analysis of residual pesticides in foods.
View here (767102 KB)

LCMS-8030/8040 Application - Simultaneous Analysis of Primary Metabolites by Triple Quadrupole LC/MS/MS Using Pentafluorophenylpropyl Column (Japan)
In recent years, LC-MS has been used for quantitative analysis of vitamin D3 due to the advantage of the sensitivity and selectivity of mass spectrometry. However one of the major drawback against precise quantification of vitamin D3 by LC/MS is an ion suppression or ion enhancement by sample matrices. In such cases, improvement of separation or removal of unexpected interferences is often required. To solve this problem, we tried to establish a new method of sample preparation to analyze vitamin D3 using two-dimensional liquid chromatography.
View here (629357 KB)

LCMS-8050 Application - An Integrated LC-MS System for Simultaneous Preparation, Separation, Detection and Quantification of Proteins and Small Molecules from Biological Fluids (SSI)
Here we report a high sensitivity LC/MS/MS method for identification and quantitation of ten artificial sweeteners in beverage samples. An ultra-small injection volume was adopted in this study to develop a very robust LC/MS/MS method suitable for direct injection of beverage samples without any sample pre-treatment except dilution with solvent.
View here (1263365 KB)

LCMS-8050 Application - Low Level Quantitation of Fluticasone and Salmeterol from Plasma Using LC/MS/MS (India)
LC/MS/MS has been increasingly employed in pharmacokinetic studies due to its specificity and sensitivity. This also allows the development of assays with minimal sample preparation. LC/MS/MS method has been developed for ultra-trace level quantitation of these molecules from plasma using LCMS-8050, a triple quadrupole mass spectrometer from Shimadzu Corporation, Japan. Ultra high sensitivity of LCMS-8050 with heated ESI source enabled development of a low level quantitation method for both these molecules with good repeatability even in presence of complex matrix like plasma.
View here (586728 KB)

LCMS-8060 Application - Multi-residue presticides analysis by LC-MS/MS using the ODS and biphenyl columns
More than a thousand different types of pesticides are being used worldwide. In recent years, due to increased awareness of food safety, the amount of pesticide residues in food are controlled by local regulatory agencies that de ne the maximum residue levels (MRLs) and enforce compliance by regular inspection. LC-MS/MS is widely employed as an analytical method for pesticide residues in the food safety because it features excellent selectivity and sensitivity even in the matrix-matched samples. As for the separation with LC, ODS has long been the first choice column chemistry but biphenyl columns are emerging as an alternative. Here we performed simultaneous LC-MS/MS analysis of 167 pesticides using both ODS and biphenyl columns for comparison.
View here (651528 KB)

Multi-residue pesticides analysis by LC-MS/MS using the ODS column and the biphenyl column
More than a thousand different types of pesticides are being used worldwide. In recent years, due to increased awareness of food safety, the amount of pesticide residues in food are controlled by local regulatory agencies that de#31;ne the maximum residue levels (MRLs) and enforce compliance by regular inspection. LC-MS/MS is widely employed as an analytical method for pesticide residues in the food safety because it features excellent selectivity and sensitivity even in the matrix-matched samples. As for the separation with LC, ODS has long been the #31;rst choice column chemistry but biphenyl columns are emerging as an alternative. Here we performed simultaneous LC-MS/MS analysis of 167 pesticides using both ODS and biphenyl columns for comparison.
View here (637548 KB)

Excellent Gradient Precision with the LPM-600 Low Pressure Quaternary Gradient Mixer
A key function of any gradient HPLC System is the ability to provide accurate and reproducible gradients. A lack of precision will result in fluctuating retention times and subsequent problems in quantitation. The Shimadzu LPM-600 Quaternary Gradient Mixer meets the requirements of precision gradients for analytical up to semi- preparative applications.
View here (87 KB)

Comparison of Semi-micro and Analytical HPLC
Development of an HPLC method can be very expensive and time consuming, especially when using the normal analytical columns and standard flowcells. Taking into account the amount of mobile phase used for these methods, the cost can increase tremendously. Shimadzu provides a solution to this problem by providing semi-micro flowcells for the SPD-10A(V), UV-Vis and RF-10A Fluorescence Detectors which can be used in conjunction with micro columns.
View here (81 KB)

Enhanced Fluorescence Sensitivity with Wavelength Programming
The Shimadzu RF-10A is a very sensitive, very flexible fluorescence detector that can be integrated with any HPLC System. Its various design features offer both high sensitivity and high selectivity. The RF-10A can perform excitation and emission wavelength scanning, and when linked via fiber optic to the SCL-10A System Controller, spectra can be viewed on the LCD display of the controller.
View here (88 KB)

HPLC Analysis of a Cold Tablet Using a 2.0 mm I.D. Column
HPLC analyses most commonly employ 4.6 mm ID columns and flow rates of 1.0 ml/min. However, the use of micro bore columns offer several advantages over the more common 4.6mm columns. The lower flow rates which are used mean that the consumption of solvent is markedly reduced.
View here (100 KB)

Updated Performance Comparison of Variable Wavelength and Photodiode Array Detectors
Shimadzu strives to achieve superior detector performance by designing high quality optical benches. To achieve this in both the UV and Vis range, dual lamp detector design is offered for both variable wavelength and PDA models. The purpose of this bulletin is to compare the relative performance of Shimadzu's UV-Vis and Photodiode Array Detectors.
View here (169 KB)

GPC Analysis of Wetting Agent
Gel permeation chromatography (GPC), is a method widely used in surfactant analysis because it separates the components based on molecular weight. Two GPC applications are presented: a metallic soap analysis and a non-ionic surfactant agent mixture analysis.
View here (99 KB)

Herbal Medicine Analysis Application
The active ingredients of Asian herbal medicines vary with their harvest times and growing region. Their quality is determined by the amount of active ingredients they contain. These medicines may contain more than one active ingredient, which heighten their effectiveness by working synergistically. It is therefore often necessary to analyze for more than one medicine or active ingredient.
View here (50 KB)

Simultaneous UV Fluorescence Quantation of Neopterine, Uric Acid, Creatinine in Urine
Neopterine in urine makes up approximately 20-50% of the total pterine, and may be clinically related to blood and liver diseases. The neopterine concentration in urine requires creatinine correction; therefore, simultaneous determination of uric acid, creatinine, and neopterine is indispensable.
View here (24 KB)

Assessing HPLC Peak Purity with Shimadzu Photodiode Detector for SPD-M10Avp
Traditionally, HPLC with a UV detector analysis generates chromatograms that present the analyte absorbance at a given wavelength as a function of the time. With the advent of the photo diode array detector, representation of the data in 3-dimensions is accomplished by adding the spectra if the analyte to the chromatogram
View here (1,484 KB)

SIL-HTc COMPETITIVE CARRYOVER PERFORMANCE ANALYZED BY LC-MS/MS: a Collaborative Study between Shimadzu Marketing Center and Covance Laboratories
Advances in the field of drug discovery have resulted in a tremendous production of potentially therapeutic compounds and, thus, another “bottleneck” downstream from synthesis to drug development.
View here (68 KB)

Prominence Application - High Speed, High Resolution Analysis (Part 33) Analysis of Gingerol and Shogaol in Ginger
Integrating spheres are frequently used for measurement of solid samples using a UV-VIS spectrophotometer. These integrating spheres are introduced here.
View here (1449226 KB)

Prominence Application - Applications Using "Prominence RF-20Axs" Fluorescence Detector (Part 6) Analysis of Bisphenol A at High Sensitivity
Here we introduce examples of analysis of cadmium in standard reference materials of powdered brown rice using the typical flame AA method, in addition to a high-sensitivity method using an atom booster.
View here (1375471 KB)

Analysis of Minor Components in Synthetic Polymers Using SEC-AccuSpot-AXIMA System (1)
Shimadzu has developed the AccuSpot automated spotter to mix the eluate from the LC with the various reagents and directly load them onto the MALDI sample plate. As a result, an automated analytical SEC-MALDI analysis system was constructed that can rapidly simplify all the processing from LC separation to MALDI-TOFMS measurement.
View here (435 KB)

Open Solution: Open Access Environment by Web Browser
As described above, there are great advantages to be realized in an open access system comprising a closed network in a laboratory that is linked to an open network in a separate office environment. The introduction of Open Solution provides an open access environment which can be utilized to its maximum to achieve great efficiencies in LC and LC/MS analysis in the analytical laboratory.
View here (1244081 KB)

Evaluation of UHPLC System Performance Under High Throughput Conditions
The use of UHPLC technology has continued to increase in LC applications as a way to reduce sample analysis turnaround times. A variety of applications in pharmaceutical and environmental areas with small particle columns will be presented that will demonstrate the throughput and performance that can be obtained with current UHPLC technology.
View here (1150973 KB)

Evaluation of MS Scanning Speeds with Ultra Fast Liquid Chromatography
Accurate mass analysis of sharp chromatographic peaks obtained by high-speed LC requires ultra-fast MS detection capabilities. In this poster, a number of high-speed separations are evaluated with MS scanning speeds of up to 15,000 u/sec with polarity switching speeds of 15 msec.
View here (756016 KB)

Nexera XR Application - High-Speed Analysis of Ultraviolet Absorbers (1)
In data sheet No. 66, a high-speed analysis example for 11 ultraviolet absorber components was shown. This data sheet shows a separation of representative four ultraviolet absorber components in shorter analysis time.
View here (339382 KB)

Nexera XR Application - High-Speed Analysis of Ultraviolet Absorbers (2)
Polymer materials such as plastics contain a lot of additives to enhance the characteristics and functionality. This chromatogram shows a high-speed analysis of 10 polymer additives.
View here (336107 KB)

Prominence Application - High-Speed Analysis of Polymer Additives (1)
In data sheet No. 68, a high-speed analysis example for 10 polymer additives was shown. This data sheet shows a separation of representative five polymer additives in shorter analysis time.
View here (341221 KB)

Prominence Application - High-Speed Analysis of Water-Soluble Vitamins
This Application News introduces the calibration curves for cadmium (Cd), copper (Cu), manganese (Mn), and lead (Pb) and the minimum limit of determination of the major elements when the booster is used.
View here (340229 KB)

Nexera XR Application - High-Speed Analysis of Alpha Acids and Beta Acids in Hops
Many different types of UV-blocking cosmetic products are commercially available to protect the skin from UV rays. This data sheet shows results of a high-speed analysis of 11 ultraviolet absorber components.
View here (345411 KB)

High-Speed Analysis of Alpha Acids and Beta Acids in Hops
Hops, a major ingredient in beer, contain components called alpha acids (humulones) and beta acids (lupulones). Through the brewing process, alpha acids are converted to iso-alpha acids (isohumulones) which are bitter components of beer. Beta acids are said to influence the bitterness balance. This data sheet shows results of a high-speed analysis of six alpha acids and beta acids.
View here (345411 KB)

HPLC Application - Ion Analysis in Drugs (Part 1) Determination of Counter-ions and Impurity Ions by Ion Chromatography
Here we introduce the simultaneous analysis of 6 related salts of PFOS and PFOA, which differ in their carbon chain length and branches.
View here (234225 KB)

HPLC Application - Application of Evaporative Light Scattering Detector (Part 8) Analysis of Terpenoids in Ginkgo Biloba
Here we present examples of analysis of counter-ions and impurity ions at micro levels in drugs using ion chromatography.
View here (272257 KB)

Prominence Application - Applications of the Prominence RF-20AXS Fluorescence Detector (Part 1) High Sensitivity Analysis of Anionic Surfactants, tert-Butylhydroquinone, and Amitrole
Here we introduce examples of high-speed analysis of tocopherols and polycyclic aromatic hydrocarbons using the Prominence RF-20AXS.
View here (258806 KB)

High Speed with High Resolution Analysis (Part 28) Analysis of α -Acids and β -Acids in Hops
Here we present an example of analysis of terpenoids in ginkgo biloba extract using the ELSD-LT II evaporative light scattering detector.
View here (245027 KB)

Prominence Application - High-Speed Analysis of Terpenoids
Ginger root is not only used as a food ingredient or spice, it is also used as a natural medicine as well. Here we present an example of high-speed analysis of 6-gingerol and 6-shogaol contained in ginger.
View here (353693 KB)

Prominence Application - High Speed Analysis of Ginkgolic Acids
Tocopherol (vitamin E) is not only used as a food additive in antioxidants and nutritional supplements, but it is also a nutrient contained in natural food materials. α-, β-, γ-, and δ- tocopherols are widely known. Here we present an example of high speed analysis of tocopherol.
View here (410942 KB)

Prominence Application - High Speed Analysis of Enrofloxacin
Ginkgo leaves contain ginkgolic acid of alkylphenols that can potentially cause allergies. Here we present an example of high speed analysis using the absorbance of ginkgolic acid and fluorescence detection. Generally, fluorescence detection has the advantages of high selectivity and less likelihood that the actual sample will be influenced by impurities.
View here (367688 KB)

HPLC Application - Determination of Chlorhexidine, Benzethonium, and Benzalkonium in Disinfectants
Phthalate is the generic term for the esters combined phthalic acid and various alcohols that are widely used as a plasticizer for various synthetic resin. Here we present the retention behavior and examples of high-speed analysis of phthalates using the ultrahigh speed Prominence UFLC system and various high-speed, high-resolution Shim-pack XR series columns.
View here (225148 KB)

Nexera XR Application - High Speed, High Resolution Analysis (Part 30) Analysis of Iso-a-Acids and a-Acids in Beer
Here we introduce examples of these analyses using the Prominence RF-20Axs fluorescence detector with the Prominence Iminoctadine Analysis System and the Prominence Carbamate Analysis System.
View here (218645 KB)

Prominence Application - Applications of the "Prominence RF-20Axs" Fluorescence Detector (Part 4) Analysis of Pesticides with a Postcolumn Derivatization System
Here we introduce analyses of mexiletine, pilsicainide, and zonisamide in serum using the ultra-high speed Prominence UFLC system and high-speed Shim-pack XR-ODS separation column.
View here (257489 KB)

HPLC Application - High Speed, High Resolution Analysis (Part 32) Analysis of Phthalates Using Shim-Pack XR Series Columns
Here we present an example of qualitative analysis of several types of polymer additives included in commercial food containers and packaging materials using the LCMS-2020.
View here (319009 KB)

High Speed Analysis of Ginkgolic Acids
Ginkgo leaves contain ginkgolic acid of alkylphenols that can potentially cause allergies. Here we present an example of high speed analysis using the absorbance of ginkgolic acid and fluorescence detection. Generally, fluorescence detection has the advantages of high selectivity and less likelihood that the actual sample will be influenced by impurities.
View here (410867 KB)

High Speed Analysis of Enrofloxacin
Enrofloxacin is a synthetic new quinolone antimicrobial agent. It is used for the treatment and prevention of pneumonia and Escherichia coli diarrhea symptoms in cows and pigs. Here we present an example of high speed analysis of enrofloxacin using fluorescence detection.
View here (367607 KB)

High Speed, High Resolution Analysis (Part 15) Analysis of Ginsenosides in Ginseng
This Application News introduces an example of the analysis of ginsenosides in ginseng using the ultra fast LC system “Prominence UFLC” with the Phenomenex Synergi 2.5 μm Polar-RP high-speed, high-resolution column.
View here (305662 KB)

High Speed, High Resolution Analysis (Part 17) Analysis of Paeoniflorin in Peony Root
This Application News focuses on paeoniflorin as one of the principle active substances in peony root, and introduces an example of analysis of paeoniflorin using the ultra high-speed LC system “Prominence UFLC” with the SPD-M20A photodiode array detector.
View here (374928 KB)

Prominence Application - RF-20A Fluorescence Detector Basics and Applications
This report addresses the problems associated with conventional LC/MS/MS systems in achieving ultra-high-speed analysis, and introduces a resolution to these problems.
View here (1628814 KB)

HPLC Application - Analysis of Electrolytic Solvents for Lithium-Ion Rechargeable Battery
Here we introduce an example of the analysis of these 3 flavonoids present in ginko bilboa leaves using the SPD-M20A photodiode array detector.
View here (956188 KB)

HPLC Application - Analysis of Hexafluorophosphate Ion in Electrolytic Solution for Lithium-Ion Rechargeable Battery
Here we introduce an example of voglibose tablet testing as specified in the Japanese Pharmacopeia, Fifteenth Edition, suing the Prominence post-column derivatizaiton system with the Prominence RF-20Axs fluorescence detector.
View here (949629 KB)

Prominence Application - Applications of the Prominence RF-20Axs Fluorescence Detector (Part 5) Analysis of Voglibose with Postcolumn Derivatization System
JIS K5602 Determination of reflectance of solar radiation by paint film is a test method used for evaluating the solar reflectance of such paint coatings. Here we introduce the measurement of solar reflectance of paint film according to this test method.
View here (1167532 KB)

Prominence Application - Applications of the Prominence RF-20AXS Fluorescence Detector (Part 7) High Sensitivity Analysis of Retinol Acetate and Retinol Palmitate
Here we used the TGA-51, and instrument capable of continuously measuring water vapor permeability relatively quickly, to measure this property in 5 types of commercially available food wrapping films.
View here (1348358 KB)

The UHPLC with the Ultimate in Resolution
Nexera supports the use of long analytical columns thereby maximizing separation efficiency thanks to a high pressure limit of up to 130MPa. In this example, two 150 mm columns with 1.8 µm particle size were connected sequentially thereby increasing Nexera’s theoretical plate number to about 70,000.
View here (225837 KB)

Ultra-High-Speed and Ultra-High-Resolution Analysis of Drug Analogs
As analogs in drug products often have similar structures, high resolution is demanded for their analysis. A long, sub-2μm column is effective in such cases but this requires a UHPLC system with high pressure tolerance, such as the Shimadzu Nexera (130MPapressure tolerance). This Application Data Sheet introduces the ultra-high-speed and ultra-high-resolution analysis of ketoprofen and its analogs.
View here (156135 KB)

Ultrafast Analysis of Aldehydes and Ketones
This document introduces an example of ultrafast analysis performed on 13 aldehyde/ketone DNPH derivatives by gradient elution using Nexera and a Phenomenex Kinetex C18 column (particle size 2.6 µm, a core-shell column where a 0.35 µm porous membrane is combined with a 1.9 µm solid core).
View here (702596 KB)

Nexera Application - High Speed, High Resolution Analysis (Part 34) Analysis of Preservatives in Cosmetics by the Nexera UHPLC System
Here we introduce an example of ultra fast analysis of resveratrol in red wine using the Nexera ultra high performance liquid chromatograph and the Prominence RF-20Axs high-sensitivity fluorescence detector.
View here (1356736 KB)

Nexera Application - High Speed, High Resolution Analysis (Part 36) Analysis of Quinolones by the Nexera UHPLC System
Here we present an example of analysis of cadmium in a standard sample (NIES No. 10a) of brown rice by the high-sensitivity electrothermal atomic absorption method using the AA-7000.
View here (1342828 KB)

Nexera Application - High Speed, High Resolution Analysis (Part 37) Analysis of Clobazam and Cibenzoline in Serum by the Nexera UHPLC System
Samples of various states can be analyzed by FTIR by selecting the appropriate accessory attachment. Here we introduce the structures and method for selecting a gas cell used for measurement of gas samples.
View here (1217291 KB)

Analysis of Hexafluorophosphate Ion in Electrolytic Solution for Lithium-Ion Rechargeable Batteries by Ion Chromatography
Lithium hexafluorophosphate is a common electrolyte used in rechargeable batteries. Here, we introduce an example of the analysis of hexafluorophosphate ion in the electrolytic solution of a lithium-ion rechargeable battery with the Shimadzu Prominence HIC-SP suppressor-type ion chromatograph.
View here (1265820 KB)

Analysis of the Decomposition Products of Lithium Hexafluorophosphate in the Electrolytic Solution of Lithium-Ion Rechargeable Batteries by Column-Switching Ion Chromatography
Here, we introduce an analysis of the decomposition products of lithium hexafluorophosphate used as the electrolytic solution in lithium-ion rechargeable batteries, in which we constructed a column-switching system using the Shimadzu Prominence HIC-SP ion chromatography system.
View here (1473391 KB)

Nexera Application - High Speed, High Resolution Analysis (Part 40) Analysis of Nucleobases, Nucleosides, and Nucleotides by the Nexera UHPLC System
Here, we introduce an example of ultra-high-speed analysis of clobazam and cibenzoline in serum using the Nexera UHPLC (Ultra High Performance Liquid Chromatography) system and the Shim-pack XR-ODSIII high-speed separation column.
View here (1299167 KB)

HPLC Application - Application of Evaporative Light-Scattering Detector (Part 10) High Speed Analysis of Glucosylceramide
This Application News introduces examples of analysis of the electrolyte solution of a lithium ion rechargeable battery and of the gas evolved from a cell that has been maintained at a high temeprature.
View here (1451748 KB)

HPLC Application - High Sensitivity Analysis of a Minor Impurity in Pharmaceuticals Using Co-Sense for Impurities System
Here, we conducted the simultaneous analysis of PFOA, PFOS, and related compounds using the LCMS-8030. The results of an environmental water monitoring study that we conducted are also presented.
View here (1340173 KB)

High Speed, High Resolution Analysis (Part 39) Analysis of Aflatoxins in Food by Nexer
Here we introduce an example of ultra-high-speed analysis of aflatoxins in food using a combination of the Prominence RF-20Axs high-sensitivity fluorescence detector and the Nexera Ultra High Performance LC system, in which the aflatoxinsB1, B2, G1 and G2 are analyzed using direct high-sensitivity fluorescence detection without conducting TFA derivatization.
View here (1506786 KB)

High Speed, High Resolution Analysis (Part 41) Performance Evaluation of Carryover Using Reserpine in Human Plasma by the Nexera UHPLC System
Here, we introduce the results of the carryover evaluation of the Nexera SIL-30AC autosampler using the Nexera UHPLC (Ultra High Performance Liquid Chromatography) System and LC/MS/MS.
View here (1271207 KB)

HPLC Application - Analysis of Dye Degradation in Dye-Sensitized Solar Cell
Here, in Application News L427, we introduce an example of improved solar cell performance achieved through high purification of a commercially available N3 dye using HPLC.
View here (1272388 KB)

Nexera XR Application - High Speed Analysis of Catechins
The WingSALDII software, provided with the Shimadzu Laser Diffraction Particle Size Analyzer, includes a Refractive Index Automatic Calculation feature that was not available in previous version of the software. Utilizing this feature, the software automatically calculates refractive indices that are appropriate for the measured sample, listing the top 5 candidates.
View here (299554 KB)

Nexera Application - Effect of Column Temperature on Organic Acid Separation
Here, we introduce a technique in which multiple organic solvents are blended online to prepare a mobile phase that is suitable for analysis.
View here (1025895 KB)

Nexera Application - Effective Method Development Using Online Blending of Organic Solvents for Mobile Phase Preparation
Here, we introduce a technique in which multiple variants of mobile phase containing different concentrations of ion-pair reagent are prepared online for use in analysis.
View here (1128929 KB)

Nexera Application - Effective Method Development Using Online Blending of Ion-Pair Reagents for Mobile Phase Preparation
Here, we introduce a technique in which multiple solutions are blended online to control and adjust the pH of mobile phases for use in analysis.
View here (1110575 KB)

Prominence Application - Simultaneous Multi-Wavelength Detection Using Fluorescence Detector
Here, using actual examples of analysis using the Shimadzu AA-7000 Atomic Absorption Spectrophotometer, we introduce factors to be considered in the analysis of metal ions in plating solution by flame atomic absorption.
View here (1076576 KB)

Prominence Application - Analysis of Melamine and Its Related Substances in Fertilizers
This article introduces an example of the analysis of dicyandiamide in fertilizer, with reference to the fertilizer test method (2012) under the supervision of the Japan‘s Food and Agricultural Materials Inspection Center (FAMIC).
View here (191975 KB)

Nexera X2 Application - i-DReC (Intelligent Dynamic Range Extension Calculator), a New Photodiode Array Detector Function; Impurity Analysis Application
Here, we introduce an example of analysis of orotic acid in yogurt by reversed-phase chromatography using a Shimadzu Prominence HPLC system.
View here (1173307 KB)

Ultra-Fast, High-Sensitivity Analysis of Degradation Products in Valsartan
The need for reliable separation and quantification of minute quantities of pharmaceutical impurities suspected of genetic toxicity continues to grow. Using the SPD-M30A high-sensitivity photodiode array detector permits high-sensitivity detection of extremely trace amounts of components. Introduced here is an example of ultra-fast, high-sensitivity simultaneous analysis of valsartan degradation products.
View here (225888 KB)

High-Speed and High-Sensitivity Analysis of Cefazolin Using SPD-M30A
Impurities present in drugs that are suspected of genotoxicity must be subjected to separation and quantitation at trace levels lower than typically required. With the SPD-M30A high-sensitivity photodiode array detector, even extremely trace level components can be detected and quantitated. Here we introduce an example of ultra-high-speed, high-sensitivity analysis of the degradation products of cefazolin.
View here (233161 KB)

Nexera X2 Application - Impurity Analysis Using the SPD-M30A Photodiode Array Detector and High-Sensitivity Flowcell
Forty analytes, and the associated internal standards for each, are included in this urinary drug confirmation panel.
View here (844240 KB)

HPLC Application - Analysis of Impurities in Pharmaceuticals Using Newly Developed Shim-Pack MAqC-ODS I column
Here, using the Shim-pack MAqC-ODS I column, we introduce an example of analysis focusing on substances that are typically included as active ingredients in over-the-counter cold medicines.
View here (921074 KB)

i-Series Application - Analysis of Sugars in Orange Juice and Grape Juice by Prominence-i and RID-10A
Here, using the New Prominent-I integrated high-performance liquid chromatograph, we introduce an example of analysis of compounds related to the abovementioned new-generation antidepressants.
View here (1032854 KB)

i-Series Application - Simultaneous Dertermination of Polycyclic Aromatic Hydrocarbons Using the Prominence-i Integrated High Performance Liquid Chromatograph
Here, we introduce an example of analysis of eight pharmaceutical substances in a workflow that is typically used for pharmaceutical synthesis confirmation analysis.
View here (975117 KB)

Nexera-e Application - Analysis of Kakkonto by Nexera-e and SPD-M30A Photodiode Array Detector (Part 1)
Here, using two analytical methods, one with the wavelength switching mode and the other using simultaneous measurement at multiple wavelengths, we introduce an example of simultaneous analysis of the 16 PAHs.
View here (1014921 KB)

i-Series Application - Investigation of Synthetic Compounds in Drug Discovery by Nexera-i and LCMS-2020 (Japan)
Here, we introduce an example of sugar analysis in juices using the Prominence-I with the RID-10A.
View here (1718644 KB)

i-Series Application - Analysis of Impurities in New-generation Antidepressants by Prominence-i
The MALDI-7090 is equipped with TrueClean an innovative source cleaning routine(2) that does not require venting of the source. TrueClean takes full advantage of the UV laser to remove any ionisation debris from the first electrode and hence prolongs analysis and maintains instrument performance.
View here (1021042 KB)

Prominence Application - Analysis of Histamine and Tyramine Using Prominence Amino Acid Analysis System
Here, we introduce an example of a faster analysis of a USP method in compliance with the new General Chapter 621 using the Nexera X2 ultra-high performance liquid chromatograph and the Shim-pack XR-ODS III high-speed analytical column.
View here (1192187 KB)

Nexera XR UHPLC 3rd Party Application - Comparing Automated vs. Manual Methods and Subsequent Recoveries of Extracted Vomitoxin from a Variety of Processed Wheat Samples (Horizon)
Vitamin D3 and related compounds were analyzed using the LCMS-8050 and APCI for high sensitivity quantitation.
View here (1073015 KB)

i-Series Application - Rapid Analysis of 2,4-DNPH-Derivatized Aldehydes and Ketones Using the Prominence-i with a Shim-pack XR-ODS Column
Here we present an example of the analysis of five anionic surfactants using the Prominence-I integrated high-performance liquid chromatograph with the RF-20Axs high-sensitivity fluorescence detector.
View here (992565 KB)

LCMS-8040 Application - Analysis of Impurities in Pharmaceutical Ingredients Using Trap-Free Two-Dimensional HPLC and Triple Quadrupole LC/MS/MS (Japan)
A method for the detection of a commercial mixture of 14 peptides from six proteins, and their corresponding heavy labeled standards, was generated.
View here (1561774 KB)

i-Series Application - Method Transfer and High-Speed Analysis of Impurities of Drug by Prominence-i
Here, we introduce an example in which we used the Kinetex 5 µm core-shell column in the Prominence-I integrated high-performance liquid chromatograph, with the aim of speeding up the analysis of a drug-related substance in accordance with criteria requirements of the European Pharmacopoeia (EP).
View here (964104 KB)

i-Series Application - Analysis of Polystyrene with Antioxidant Additive Using Prominence-i GPC System
In this Application News, we introduce an accurate identification method for typical steroidal and non-steroidal anti-inflammatory drugs using multiple reference ion ratios, in addition to an example of high-sensitivity measurement.
View here (1001124 KB)

i-Series Application - Analysis of Nivalenol and Deoxynivalenol in Wheat Using Prominence-i
Ethylene is a type of plant hormone. It promotes the growth of fruits and vegetables, and suppresses the sprouting of potatoes. This experiment details the analysis of ethylene produced by apples.
View here (1108754 KB)

Prominence Application - Analysis of Biomass Using Organic Acid Analysis System
The detector component of the new Prominence-I integrated high-performance liquid chromatograph incorporates a temperature control function for both the flow cell component and the optical system. Here, good repeatability was obtained despite the susceptibility of UV detection in the short wavelength region due to environmental temperature fluctuations.
View here (968346 KB)

Nexera UC Application - Using the Nexera UC Online SFE-SFC-MS System to Analyze Residual Pesticides in Agricultrual Products (Japan)
This article describes an example of using the Nexera UC online SFE-SFC-MS system to analyze residual pesticides in agricultural products
View here (2086357 KB)

Prominence Application - Analysis of Melamine and Its Related Substances in Fertilizers
This article describes an example of pretreating and analyzing melamine and its related substances, namely ammeline, ammelide, and cyanuric acid, in fertilizer, in accordance with the testing methods supervised by the Food and Agricultural Materials Inspection Center (FAMIC) in Japan for fertilizers and other substances
View here (92971 KB)

LCMS-8050 Application - A High Sensitivity LC/MS/MS Method with QuEChERS Sample Pre-Treatment for Analysis of Aflatoxins in Peanut Butter Samples (Singapore)
A atoxins are metabolites produced by fungi (Aspergillus avus and Aspergillus parasiticus) in high humidity environment in crops such as maize nuts and processed food. A atoxin contamination in food is monitored with strict regulations worldwide due to high toxicity of the compounds. Recently, several media reports revealed the exceed levels of aflatoxins found in peanut butters in the USA and Taiwan. Aflatoxins in food have been analyzed by LC/MS/MS using various sample pre-treatment methods. We describe a high sensitivity LC/MS/MS method for quantitative analysis of aflatoxins in peanut butters using QuEChERS sample pre-treatment procedure, as opposed to the use of immunoaffinity column or other methods for sample pre-treatment which are more expensive and tedious. High sensitivity and good recoveries were achieved using this LC/MS/MS method.
View here (205522 KB)

LCMS-8050 Application - High throughput quantitation for hterapeutic drug monitoring with Open access LC/MS/MS system (Japan)
In this paper, we introduce four research use only LC/MS/MS methods for therapeutic drug monitoring (TDM), mycophenolic acid, sunitinib and axitinib, voriconazole, itraconazole. TDM is indispensable for managing drug dosage based on the drug concentration in blood in order to conduct a rational and ef cient drug therapy. Liquid chromatography coupled with tandem quadrupole mass spectrometry (LC/MS/MS) is increasingly used in TDM because it can perform selective and sensitive analysis by simple sample pretreatment. In the field of TDM, it is necessary to measure the specimen such as plasma or serum quickly after suitable pretreatment and report the precise result. LC/MS/MS system with a simple and user-friendly interface can provide a streamlined work flow and reduce the load of analysts. We developed high-throughput LC/MS/MS methods for TDM with a new data acquisition and processing software.
View here (422861 KB)

High Sensitivity Porphyrin Analysis by Fluorescence Detection using R928 PMT
The analysis and quantitation of porphyrins for diagnosis has been, until recently, very complex and time consuming. HPLC has become a very effective analytical method, since it can separate and quantitate individual porphyrins very rapidly. The Shimadzu LC-10A System with the RF-10A Fluorescence Detector offers both high sensitivity and high selectivity in the analysis of porphyrins. The sensitivity is enhanced by using the optional Photomultiplier Tube R928-08.
View here (89 KB)

Analysis of Clean In Place 150 Residues on Process Equipment Using UV Detection
The pharmaceutical industry has recently become concerned with the efficacy of cleaning procedures not only to remove active drug, but also to remove the products used to clean the process equipment. At Schein Pharmaceutical in Carmel, New York, the robotics department has developed a comprehensive program to validate the efficacy of current cleaning protocols. This program incorporates the use of a Shimadzu LC-10A Series HPLC System to detect trace amounts of cleaning agents
View here (90 KB)

Prominence Application - High Speed with High Resolution Analysis (Part 28) Analysis of α -Acids and β -Acids in Hops
Here, we introduce an example of analysis of ferulic acid in berry juice using a system constructed specifically for efficient handling of this application. Shimadzu’s Prominence UFLC ultra fast LC system forms the base of the system, which also includes a column switching system comprising the first dimension separation column, a trap column, and the second dimension separation column.
View here (245027 KB)

Prominence Application - Applications of the Prominence RF-20AXS Fluorescence Detector (Part 2) High-Speed Analysis of Tocopherols and Polycyclic Aromatic Hydrocarbons
Here we introduce an example of high-speed analysis of α-acids and β-acids in hops using the Prominence UFLCXR ultra fast, high resolution LC system with a high-speed, high-resolution column.
View here (310796 KB)

Impurity Analysis by High-sensitivity UV Detector
Analysis of impurities can be a challenging task especially whenthe main ingredient needs to be assayed at the same time, which requires a wider dynamic range and lower baseline disturbances. With an extra wide dynamic range, temperature-controlled flow cell and a stray-light correction function, both SPD-20A UV and SPD-M20A Photo Diode Array detectors offer a high level of stability, sensitivity andlinearity for a confident analysis. The 100 Hz sampling of the SPD-20A/M20A ensures peak information can be captured without loss of resolution and exploits the full potential of ultra-fast LC columns.
View here (220992 KB)

Nexera Application - High Speed, High Resolution Analysis (Part 38) Analysis of Artificial Colorings with the Nexera UHPLC System
Here we introduce an example of ultra-high-speed analysis of aflatoxins in food using a combination of the Prominence RF-20Axs high-sensitivity fluorescence detector and the Nexera Ultra High Performance LC system, in which the aflatoxins B1, B2, G1, and G2 are analyzed using direct high-sensitivity fluorescence detection without conducting TFA derivatization.
View here (2157617 KB)

Long-term Automated HPLC Analysis of Microdialysis Samples from Multiple Freely Moving Animals
Online microdialysis integrated with real-time HPLC analysis is a powerful tool for providing information on the circadian pacemaker, especially in combination with molecular and pharmacological tools. Other applications of this system are certainly possible for the long-term in-vivo analysis of various biological substances in freely moving animals. To access the full issue of LC World talk, please click <a href="http://www2.shimadzu.com/lc_worldtalk/" target="_blank">here</a>.
View here (604161 KB)

Impurities Analysis in Pharmaceuticals: FDA Regulations on Genotoxic Impurities in Pharmaceuticals
The FDA draft guidance was issued to cover the verification of the genotoxicity and carcinogenicity of ultra-trace impurities in new pharmaceuticals, investigational new drugs, and generic pharmaceuticals by structural analysis of ultra-trace impurities. This demands structural analysis of ultra-trace impurities in a 200 mg daily drug dose at approximately 150 times lower levels than under the ICH guidelines. LCMS-IT-TOF analysis, which provides precise mass measurement and MSn spectra, is an effective method for the structural analysis of ultra-trace impurities. To access the full issue of LC World talk, please click <a href="http://www2.shimadzu.com/lc_worldtalk/" target="_blank">here</a>.
View here (1118267 KB)

HPLC Application - Simultaneous Determination of Drug Compound and its Counter-ions by RPLC×IC
The United States Pharmacopoeia has established guidelines for determining system suitability and established the acceptance of Water For Injection (WFI) purposes and Purified Water (PW) (USP Method <643>). Shimadzu’s TOC-LC*H analyzer is perfectly adapted to meet the requirements of USP Method <643>. The TOC-LC*H analyzer utilizes 680°C heat and platinum catalyst to provide a lower maintenance instrument with a detection limit of 0.0040 mg per liter.
View here (1192440 KB)

HPLC Application - Amino Acid Analysis System Analysis Handbook
In this study, we found that a methionine residue is modified in a mutant of another heme protein. However, among the peptide fragments obtained by the peptidase digestion of the modified protein, the two peptides which contain methionine was constructed with the same set of amino acids and exhibited the same molecular weight. We identified the modified amino acid in this mutant protein by using LC/MS/MS.
View here (1643178 KB)

Nexera Application - Evaluation of LC-MS Data under Ultra-High Throughput Conditions (SSI)
We developed an ultra fast UHPLC-MS-MS method for analysis of carbendazim in orange juice using a new high speed autosampler, the Nexera SIL-30ACMP in tandem with a newly developed high sensitivity triple quadrupole mass spectrometer, the LCMS-8040.
View here (1474526 KB)

Improved R&D Efficiency Through Speedier Method Development (3)
Method scouting is the search for analytical conditions (column, mobile phase, and gradient settings) that optimize an LC separation. When used with a UHPLC (ultra high performance LC) system, the time to produce a robust, validated method is greatly shortened, which leads to an increased interest in and application of UHPLC systems for method development. In this report, we introduce an example of such scouting using the Nexera Method Scouting System together with its specialized Method Scouting Solution software to conduct a search for simultaneous analytical conditions to be used in analysis of 13 cephem antibiotic substances.
View here (700326 KB)

LCMS-8040 Application - Lipids Analysis by 2 Dimensional LC Coupled with Triple Quadrupole MAss Spectrometer (Japan)
Fragmentation Outcome Modelling is a new approach to the prediction of CID fragment ions and has been successfully applied to a series of pharmaceutical structures generating complete fragmentation including rearrangement mechanisms. This expert system uses a series of prediction models that encapsulate the outcome of fragmentation mechanisms that could result in the breaking of one, two or three bonds. In this paper, midazolam and its 1-hydroxy and 4-hydroxy metabolites were used as test compounds to highlight the advantages of fragmentation outcome modelling compared to other commercially available fragmentation prediction software products.
View here (904427 KB)

Nexera-e Application - 2-Dimensional Separation of Triacylglycerols in Borago Officnalis Using the Shimadzu 2D-LC System Coupled to an Evaporative Light Scattering Detector and IT-TOF
In this paper we describe the analytical protocol developed by Mass Spectrometry, Clinical Chemistry and Pharmacology Lab of Meyer Children’s Hospital to measure amino acids and acylcarnitines from dried blood spot samples using the LCMS-8040 high-performance liquid chromatograph triple quadrupole mass spectrometer.
View here (2577189 KB)

Nexera-e Application - Comprehensive Two-dimensional Liquid Chromatography/Triple Quadrupole Mass Spectrometry: the Perfect Marriage (Japan)
This technical report describes a novel LC×LC/PDA/MS/MS instrument, capable of extremely high-resolution power, as well as targeted and untargeted analysis, that was successfully applied to the characterization of the polyphenol content a red wine sample.
View here (1741747 KB)

Nexera-e Application - Continuous vs. Segmented Second Dimension System Gradients for Comprehnsive Two-dimensional liquid Chromatography of Sugarcane (Saccharum spp.) (Japan)
This technical report describes a novel LC×LC/PDA/MSMS instrument, capable of extremely high-resolution power, as well as targeted and untargeted analysis, simultaneously. The system was successfully employed for the characterization of the native carotenoids in red chili pepper, also allowing for quantification of beta-carotene, at sub-ppm level.
View here (1080228 KB)

HPLC Application - Analysis of Vitamin D3 in Dietary Supplements by 2-dimensional LC system (Japan)
The requirement for universal, reliable and fast methods for drug determination in water is steadily increasing. Highly sensitive triple-quad-MS systems are suitable tools for the analysis of residues in ground-, surface- and wastewater, but development of a simple, rapid and robust method for simultaneous measurement of trace levels of various different classes of analytes in complex matrices is a challenge.
View here (504839 KB)

2-Dimensional separation of triacylglycerols in Borago officinalis using the Shimadzu 2D-LC System coupled to an Evaporative Light Scattering Detector and IT-TOF
Triacylglycerols (TAGs) are the major components of fats and oils from animal and vegetable sources. The high number of Fatty Acids combinations in the glycerol backbone can create an intricate pattern of compounds, difficult to separate under monodimensional HPLC analysis. This Technical Report demonstrates the potential of comprehensive two-dimensional liquid chromatography (LCxLC) using the Shimadzu 2D-LC system with both Evaporative Light Scattering detector and mass spectrometer (IT-TOF) for the analysis of triacylglycerols in a complex sample.
View here (960546 KB)

Comprehensive two-dimensional liquid chromatography for determination of polyphenols in red wines
A comprehensive two-dimensional liquid chromatography method was developed and applied to to determination of polyphenols in red wines. To fulfil such a task, a micro cyano and a partially porous octodecylsilica columns were employed in the first and the second dimension, respectively in combination with photodiode array and mass spectrometry (LC×LC-PDA-MS) detection. To increase the peak capacity values by using RP modes in both dimensions, a comparison of a conventional full-in-fraction and shifted second gradient gradient was carried out. The separation capabilities of the comprehensive LC approaches tested allowed the analysis of such a complex natural sample without any pre-treatment to effectively reduce the interferences coming from the matrix.
View here (811223 KB)

i-Series Application - Chromatographic Performance of the i-Series Integrated LC coupled to LCMS-8050 (SSI)
In Application News No. L452, the analysis of a pyridylamino (PA)-glycan using a fluorescence detector was introduced. Here, the analysis of a 2-aminobenzamide-labelled glycan (2-AB glycan) is introduced. As in Application News No. L452, the world’s highest sensitivity fluorescence detector, the RF-20Axs, was used for detection
View here (463327 KB)

Authenticity & Adulteration, Food Beverages & Other Consumer Products, Health, Dietary, Nutraceutical & Supplements
Here, carotenoids extracted from red chili pepper were subjected to two-dimensional analysis, in which mico-scale separation was conducted in the first stage using normal phase conditions, and separation using reversed phase conditions was tried in the second dimension. For detection, a combination of a photodiode array (PDA) connected to the LCMS-8030 triple quadrupole mass spectrometer was used. Because the separation modes, normal and reversed phases, differ in the first and second dimensions, this might be considered a two-dimensional LC method by which the greatest orthogonality possible is obtained.
View here (2261417 KB)

LCMS-2020 Application - Determination of Molecular Weight of Synthetic Peptides by LC/MS Using Multi-Charged Ion Analysis Software (Japan)
Here, Asp-His-Pro-Asn-Pro-Arg (DHPNPR), a synthetic product consisting of the N-terminal partial fragment of the C-type natriuretic peptide (OvCNP) that is present in platypus venom, was measured using the Nexera-I and LCMS-2020. Multi-Charged ion analysis software was then used to conduct molecular weight confirmation and impurity analysis. This application News introduces the results of the analysis
View here (1100507 KB)

LCMS-8030 Application - Comprehensive Two-dimensional Liquid Chromatography/Triple Quadrupole Mass Spectrometry: The Perfect Marriage (Japan)
This novel system combines the separation capabilities of comprehensive two-dimensional liquid chromatography (LC×LC), and the specificity and sensitivity of triple quadrupole mass detection (MSMS). The hyphenation of the techniques generates a powerful analytical system, capable of extremely high-resolution power, as well as targeted and untargeted analysis, simultaneously. The so-called selected reaction monitoring (SRM) mode in fact enhanced selectivity, reducing sample consumption and the need for tedious clean-up procedures, specifically for beta-carotene quantification in a red chili pepper extract.
View here (635001 KB)

LCMS-8030 Application - Comprehensive Two-dimensional Liquid Chromatography for Determination of Polyphenols in Red Wines (Japan)
A comprehensive two-dimensional liquid chromatography method was developed and applied to the determination of polyphenols in red wines. To full such a task, a micro cyano and a partially porous octadecylsilane columns were employed in the rst and the second dimension, respectively in combination with photodiode array and mass spectrometry (LC×LC-PDA-MSMS) detection. To increase the peak capacity values by using RP modes in both dimensions, a comparison of a conventional full-in-fraction and shifted second dimension gradient was carried out. The separation capabilities of the comprehensive LC approaches tested allowed the analysis of such a complex natural sample without any pre-treatment to effectively reduce the interferences coming from the matrix.
View here (651054 KB)

LCMS-IT-TOF Application - 2-Dimensional Separation of Triacyclgycerols in Borago Officinalis Using the Shimadzu 2D-LC System Coupled to an Evaporative Light Scattering and IT-TOF Detection (Japan)
In this technical report, we investigated a comprehensive two-dimensional LC system, comprised of a cation exchange micro-column loaded whith silver ions (150 mmL. × 1.0 mmI.D.; 5.0 µm) in the first dimension (D1) and a partially porous column (50 mmL. × 4.6 mmI.D.; 2.7 µm) in the second dimension (D2), in combination with an evaporative light scattering detector (ELSD) and IT-TOF mass spectrometer, for the analysis of TAG fraction of a borage oil sample.
View here (610115 KB)

Four-Channel Vacuum Degasser-Maximum Degassing Efficiency in an Ultra-Compact Design.
Eliminates helium degassing to save time and money/Fast, efficient degassing from up to 4 solvent channels/Steady, Self-Maintaining Vacuum/Metal-Free Bioinert Composition and Advanced Self-Diagnostics
View here (139 KB)

CLASS-VP<SUP>TM</SUP> - New Tools for Better Solutions
CLASS-VP<SUP>TM</SUP> is a multi-tasking chromatography data acquisition and instrument control system operating under Microsoft Windows<SUP>TM</SUP>.
View here (81 KB)

CLASS-VP<SUP>TM</SUP> - New Tools for Better Solutions
A New Program with New Tools, to Make Chromatographic Data Processing More Powerful Than Ever acquisition and instrument control system operating under Microsoft Windows<SUP>TM</SUP>.
View here (83 KB)

TOGAS - Transformer Oil Gas Analysis System
The analysis of gas in transformer oil is not a new requirement. Care and maintenance of expensive transformers has been facilitated by routinely sampling the transformer oil and determining the concentration of various gases.
View here (119 KB)

Vitamin Analysis with an Integrated HPLC System
In the last few years, vitamin supplements have become increasingly important to consumers who are concerned about maintaining the recommended daily allowances of certain vitamins, or who are focusing on specific vitamins that show promise of disease prevention or other health benefits.
View here (22 KB)

Steroid Analysis with an Integrated HPLC System
Steroids are a structurally unique type of drug, most commonly used for anti-inflammatory purposes. In general, they can be used to treat asthma, arthritis, allergies, and may be combined with other medications to help prevent the body from rejecting transplanted organs.
View here (15 KB)

The HPLC Analysis of Black Cohosh Using an INA Method
The Institute for Nutraceutical Advancement (INA) is a consortium of research and commercial laboratories whose mission is the development of standardized methods for the analysis of natural products. A myriad of nutraceutical products is available to health-conscious consumers.
View here (34 KB)

ELSD and UV - Complementary Detectors
Reversed phase HPLC with UV detection at 210nm has been used to determine constituents in commercial Stevia products, but the methodology is limited in its ability to separate all components of interest, especially when higher order oligosaccharides are present.
View here (178 KB)

Analysis of Berberine in Crude Drugs
The SPD-M6A, employing a photodiode array sensor, is capable of storing data in the wavelength range of 195 nm to 870 nm, while observing the chromatogram at two wavelengths selected arbitraily in real time.
View here (101 KB)

High Sensitivity and High Selectivity Analysis of Ammonia with HPLC.
Quantitative measurement of ammonia is being performed in a wide field, including quality control, measurement in working environment, monitoring of environmental atmosphere, as well as in the field of biochemistry.
View here (98 KB)

Analysis of Hair Tonics
Shown in this application note is a chromatogram of Hinokitiol standard, and one in hair tonic. In this analysis, the hair tonic was diluted with methanol and a sample of it was injected into the HPLC for analysis.
View here (65 KB)

Rapid and Sensitive Analysis of Aluminum Ions using On-column Derivatization (Part 2) - Application to the Analysis of luminum Ions in Total Parenteral Nutrition Solutions
View here (73 KB)

AXIMA-TOF 2 Simultaneous Protein Identification and Relative Quantification of Complex Mixtures using iTRAQ. methodology, LC-MALDI and AXIMA-TOF2.
View here (178 KB)

Applications of Prominence RF-20AXS Fluorescence Detector - Analysis of Saccharides Using Post-Column Derivatization System
Here we present some examples of analyzing saccharides using the reducing sugar analysis system (anion exchange mode) with the Prominence RF- 20AXS.
View here (315761 KB)

Ion Analysis in Drugs - Determination of Counter-ions and Impurity Ions by Ion Chromatography
Here we present examples of analysis of counter-ions and impurity ions at micro levels in drugs using ion chromatography.
View here (234225 KB)

High Sensitivity Analysis of a Minor Impurity in Pharmaceuticals Using Co-Sense for Impurities System
Here, we introduce an example in which the Co-Sense for Impurities System is applied to a drug impurity analysis, making it possible to conduct measurement quickly and easily through automation of the sample preparation.
View here (1340173 KB)

Improvement of Dye-Sensitized Solar Cell Efficiency ThroughHigh Purification of Dye
Here in Application News L427, we introduce an example of improved solar cell performance achieved through high purification of a commercially available N3 dye using HPLC.
View here (1449206 KB)

HPLC Application 3rd party - Triglycerides by SFC
The theme of this UV TALK LETTER is the instrument validation of UV-VIS spectrophotometers. Instrument validation is essential for determining the condition of your instrument. Here, we will give details of what validation is and how to do it.
View here (48929 KB)

Post-Column pH Buffered Electric Conductivity Detection of Organic Acids with Ultra High-Performance Liquid Chromatography
Here, we introduce an example of ultra fast simultaneous analysis of organic acids in which this detection technique was applied to organic acid separation by UHPLC.
View here (1298525 KB)

LCMS-2020 Application - Quantitative Analysis of Carbohydrates by LC/MS (Japan)
Here we introduce an example of high-sensitivity measurement of phosphorylated peptides using the AXIMA Resonance combined with a μFocus plate.
View here (1219813 KB)

LCMS-IT-TOF Application - Analysis of Drug Degradants by LC/MS (Japan)
The Axima Performance system for two-dimensional electrophoresis used here is an extremely effective tool for posttranslational modification analysis, as demonstrated in these results of analysis of carbonylated proteins as one type of oxidative stress to proteins.
View here (272103 KB)

Improved R&D Efficiency Through Speedier Method Development (1)
Various approaches are available for improving the efficiency of analytical method development. The introduction of high-speed analysis into the method development process for LC and LC/MS is one approach that can directly enhance development efficiency by simply speeding up chromatographic evaluation.
View here (669143 KB)

Application of Metabolomics Techniques using LC/MS and GC/MS Profiling Analysis of Green Tea Leaves
This Application Note presents the profiling of green tea leaves as an example of one application of the metabolome analysis technique using LC/MS and GC/MS. A search of the substances believed to play roles in product quality was conducted, and a quality prediction model was constructed based on the results.
View here (677759 KB)

MALDI-Performance Application - Analysis of Methylglyoxal-Modified Heat Shock Protein 27 Using LC-MALDI System (Japan)
Here we introduce examples of high-sensitivity analysis of retinol acetate and retinol palmitate, in addition to ultra-high speed analysis of retinol palmitate using the Prominence RF-20Axs fluorescence detector.
View here (1295257 KB)

LCMS-8030/8040 Application - Analysis of Golf Course Pesticides Using Triple Quadrupole LC/MS/MS (LCMS-8030) (Japan)
In this issue, we present an example of ultra-high-speed analysis using the Nexera UHPLC (Ultra High Performance Liquid Chromatography) System.
View here (1308603 KB)

LCMS-8030/8040 Application - Analysis of PFCs in Environmental Water Using Triple Quadrupole LC/MS/MS (LCMS-8030) (Japan)
Here, we introduce an example of analysis of polyethylene terephthalate as a recycled polymer using precipitation for the rough separation of the oligomers together with SEC-MALDI.
View here (1428778 KB)

LCMS-8030/8040 Application - Analysis of Geniposidic Acid and Chlorogenic Acid in Tochu Tea Using a Triple Quadrupole LC/MS/MS [LCMS-8030] (Japan)
Here, we describe the precursor ion scan in the search for active ingredients in tochu tea using the LCMS-8030.
View here (1005460 KB)

LCMS-8030/8040 Application - Analysis of 3-MCPD Fatty ACid Diesters in Palm Oil Using a Triple Quadrupole LC/MS/MS [LCMS-8030] (Japan)
Here, we introduce an analysis of geniposidic acid and chlorogenic acid in tochu tea using a triple quadrupole mass spectrometer.
View here (997585 KB)

ICP Application - Analysis of Additive Elements in Lubricating Oil using ICPE-9000
The LC/MS(/MS) method eliminates the solvent extraction and derivatization steps currently conducted as part of the GC/MS method, and requires only the direct injection of the sample into the LC/MS.
View here (928943 KB)

LCMS-8030/8040 Application - Analysis of Malachite Green Using a Triple Quadrupole LC/MS/MS [LCMS-8030] (Japan)
Here, using the LCMS-8030, we optimized methods for the simultaneous multi-residue analysis of 43 pesticides, and report the results of the analysis of actual vegetable extracts (paprika and leek) in solution.
View here (796762 KB)

LCMS-8030/8040 Application - Analysis of Haloacetic Acids in Tap Water Using LC/MS/MS [LCMS-8030] (Japan)
Here, we show the quantitative analysis of malachite green and leucomalachite green using the LCMS-8030. In addition, we report the results of spiked-recovery measurements conducted using a salmon extract solutions as an actual sample.
View here (976402 KB)

LCMS-8030/8040 Application - A Fully Automated Multiple Injection On-Line SPE-LC-MS/MS Method for Analysis of Trace Level Drug Residues in Water (Singapore)
In this study, we propose a rapid and systematic methodology to quickly optimize HPLC mobile phase recipe from a MS sensitivity point of view.
View here (706875 KB)

LCMS-8030 Application - Sensitive detection and quantification of hydrogen sulfide as a gasotransmitter by combining monobromobimane-based derivatization to triple quadrupole LC/MS/MS (Japan)
In this study we developed a rapid online-SPE-LC system coupled with a high-speed triple quadrupole mass spectrometer for the simultaneous determination of phthalate di- and mono-esters to trace levels.
View here (248801 KB)

LCMS-8030/8040 Application - Fast LC-MS/MS Screening Method for Antipsychotics with Data Dependent Analysis for Untargeted Analtes (SSI)
In this study, we report a developed analytical system for hydrophilic metabolite using ion-pare chromatography with a high-speed triple quadrupole mass spectrometer.
View here (900517 KB)

LCMS-IT-TOF Application - Development of an LC-Based Metabolomic Approch for Polar Compounds in Brewage Samples using Fast Polarity Switching TOFMS Acquisition (Japan)
In this study we show differential analysis of similar structured sulfenamide-based vulcanizing accelerators produced by different manufacturers using high mass accuracy MSn and multivariate statistical technique.
View here (497788 KB)

LCMS-8040 Application - Profiling of Triacylglycerides Present in Edible Oils Consumed in India Using LC/MS/MS (India)
Medicinal plants have played an important role in drug discovery with many pharmaceutical products originating from plant. Isolation and characterization of antibacterial compounds is still relevant because of continuous development of resistance of bacteria to antibiotics.
View here (177975 KB)

LCMS-8040 Application - Rapid and Robust Analysis Method for Quantifying Antidepressants and Major Metabolites in Human Serum by UHPLC-MS/MS (Netherlands)
Here, we utilise the improved response from micro flow LC to achieve the required low limits of detection for over one hundred pesticides in infant food. Initial validation results are presented for the micro flow LC method, in addition to robustness data.
View here (347666 KB)

LCMS-8040 Application - LC-MS Analysis of Amino Acids on a Novel Mixed-Mode HPLC Column (Non-derivatized) (SSI)
In this application more than 50 samples of different matrices were split and analysed by the Shimadzu GCMS-TQ8030 triple quadrupole mass spectrometer and the Waters Autospec GCHRMS.
View here (1047691 KB)

LCMS-8040 Application - High Sensitivity Analysis of Acrylamide in Potato Chips by LC/MS/MS with Modified QuEChERS Sample Pre-Treatment Procedure (Asia Pacific)
We have developed a single, UHPLC column-based LCMS method to analyze the TAG components in commercial chocolate and chocolate-like products.
View here (229822 KB)

LCMS-8040 Application - An LCMS Method for the Detection of Cocoa Butter Substitutes, Replacers, and Equivalents in Commercial Chocolate-like Products (SSI)
This study was aimed to elucidate the plasma matrix effect on the quantification of these three cathinones by LC-MS/MS. We developed LC-MS/MS methods that utilize standard addition without internal standard. A mixture of cathinone and mephedrone in plasma was analyzed.
View here (244644 KB)

LCMS-8030 Application - Analysis of Cathinones in Plasma Using LC-MS/MS (SSI)
This report illustrates the simultaneous analysis of 36 veterinary drugs measured in 15 minutes using the Shimadzu LCMS-8050 Ultra Fast Triple Quadrupole Mass Spectrometer, featuring ultrafast polarity switching. The polarity switching speed of the LCMS-8050 is just 5 milliseconds.
View here (139069 KB)

LCMS-8050 Application - Highly Sensitive Quantitative Analysis of Felodipine and Hydrochlorothiazide from Plasma using LC/MS/MS (India)
This data sheet illustrates high-speed quantitative analysis of 16 anti-epileptic drugs (AEDs) using the Shimadzu UFMS Triple Quadrupole Mass Spectrometer, LCMS-8050.
View here (480711 KB)

LCMS-8050 Application - Simultaneous Analysis of 36 Veterinary Drugs Using Triple Quadrupole LC/MS/MS (Japan)
In this study, we developed a high-speed and sensitive method for measurement of seventeen antiepileptics in plasma by UHPLC coupled with tandem quadrupole mass spectrometer.
View here (219111 KB)

LCMS-8050 Application - High Speed Analysis of Haloacetic Acids in Tap Water Using Triple Quadrupole LC-MS/MS (Japan)
This application illustrates a drug screening method in putrefied human pleural fluid using the Shimadzu UFMS triple quadrupole mass spectrometer, LCMS-8050.
View here (418578 KB)

LCMS-8050 Application - High Speed Quantitative Analysis of Anit-Epileptic Drugs Using Triple Quadrupole LC/MS/MS (Japan)
This data sheet illustrates results from a high speed method acquired using a LCMS-8050 triple quadrupole mass spectrometer coupled with a Nexera X2 UHPLC.
View here (328695 KB)

LCMS-8050 Application - Highly Polar Pesticide Analysis in Food Samples by LC-MS/MS (UK)
Here, we introduce an example in which the newly developed “Shim-pack MAqC-ODS I” column is used to conduct simultaneous analysis of water-soluble vitamins without the addition of ion-pair reagents to the mobile phase.
View here (678107 KB)

LCMS-8040 Application - Analysis of Phenols in Drinking Water Using Triple Quadrupole LC/MS/MS (Japan)
A method for rapid quantitation of various cannabinoids utilizing a Nexera X2 UHPLC coupled to an LCMS-8040 triple quadrupole mass spectrometer was developed.
View here (903378 KB)

LCMS-8050 Application - Simultaneous Analysis of Culture Supernatant of Mammalian Cells Using Triple Quadrupole LC/MS/MS (Japan)
Here, we introduce an example of analysis of the polysorbate 80 surfactant, widely used as an additive to prevent protein aggregation and adsorption, and to increase protein solubility in a protein formulation.
View here (905650 KB)

High-Speed, High-Sensitivity Analysis of Drugs in Plasma Using Triple Quadrupole LC/MS/MS (LCMS-8040)
This Application News introduces examples of high-speed, high-sensitivity analysis of four drug substances, including the endothelin receptor antagonists (ERA) bosentan and ambrisentan, and the phosphodiesterase-5 (PDE-5) inhibitors sildenafil and tadalafil. All of these substances are used as therapeutic agents for the treatment of pulmonary arterial hypertension (PAH), and the analysis was conducted by LC/ MS/MS using ESI in positive mode.
View here (1019546 KB)

Simultaneous Analysis of Hydrophilic Metabolites Using Triple Quadrupole LC/MS/MS
In this data sheet, tributylamine was used as an ion pair reagent. It illustrates simultaneous analysis of hydrophilic metabolites using a Shimadzu UFMS triple quadrupole mass spectrometer, the LCMS-8040, with a ready-to-use “LC-MS/MS method package for Primary Metabolites”.
View here (321564 KB)

LCMS-8040 Application - Simultaneous Analysis of Nine Sweetners Using Triple Quadrupole LC/MS/MS (Japan)
This article presents a simultaneous analysis of nine sweeteners including both specified additives and unspecified additives, using the LCMS-8040 high-performance liquid chromatograph-triple quadrupole mass spectrometer
View here (893799 KB)

LCMS-8060 Application - Separation and Quantitation of Oxysterol Compounds Using LC-MSMS (SSI)
A mixture of 16 oxysterols and cholesterol related compounds were separated using a Shimadzu Nexera UHPLC and analyzed by a Shimadzu LCMS-8060 system. Detection and quantitation limits were obtained using APCI, ESI, and Dual Ion (DUIS) sources.
View here (599006 KB)

Analysis of Anions in Soil
For the analysis of inorganic ions, a special ion chromatograph or the reversed phase ion pair method by a HPLC is applied.
View here (52 KB)

Analysis of a drug in plasma using ON-LINE pretreatment method to remove proteins for LC-MS
View here (118 KB)

Confirmation of Aureomycin and Urea in Livestock Feed Mix by LC/MS
A livestock feed was analyzed to confirm the presence of urea and aureomycin, 7-cholrotetracycline
View here (224 KB)

High-Speed Analysis of Chlorogenic Acid
View here (282 KB)

High-Speed Analysis of Artificial Colorant
View here (311 KB)

High-Speed Drug Analysis
View here (317 KB)

LC-MS Analysis of Carbohydrates Using Post ColumnAddition of Solvent for Improved Ionization Efficiency
Typically, in the HPLC analysis of saccharides, two different modes of chromatography can be used: aqueous normal phase, or ligand exchange mode. Due to the difficulty in completely separating all of the saccharides, these are used in a complementary manner. Since salts that are not easily volatilized cannot be used in LC-MS analysis, the suitability of the HPLC conditions for LC-MS analysis depends on the choice of the mobile phase. Because acetonitrile - water (or ammonium acetate in water) is generally used as the mobile phase in the aqueous normal phase mode, and only water is used as the mobile phase in the ligand exchange mode, these can be considered suitable mobile phases for LC-MS analysis. While these conditions are very suitable for the HPLC separation of mixed carbohydrates, there can be difficulty in observing an ion which up to then has been easily confirmed, or there may be a loss of sensitivity due to the separation column or the HPLC conditions.
View here (568 KB)

Quantitative Analysis of Carbohydrates by LC/MS
Here we introduce examples of quantitative analysis of carbohydrates in foods using post-column solvent addition.
View here (1219813 KB)

Drugs of Abuse: Benzodiazepines and Barbiturates
A rapid, accurate, and reliable LC-MS-MS method was developed for the determination of 21 controlled substances in urine.
View here (1346146 KB)

Designer Cannabinoids
A rapid LC-MS-MS method for determination of designer cannabinoids in smokeable herbs was developed.
View here (1132832 KB)

Mycotoxins
An extremely fast LC-MS-MS method for the determination of mycotoxins and other untargeted chemical threats was developed.
View here (1229865 KB)

LCMS-8030/8040 Application - Simultanerous Analysis of Alkylphenol Ethoxylates using Ultra-High Speed LC-MS/MS (Japan)
Here we introduce a novel LC/MS method using gel filtration chromatography (GFC) and single quadruple mass spectrometer with APCI interface for separation and detection of a total of sixteen carbohydrates (sugars and sugar alcohols) and three artificial sweeteners with pure water as the mobile phase, the results of the method were applied to food samples and a mouth rinse product. It is known that sugar molecules are not easily to be ionized on LCMS interface and the pure water mobile phase is not a favourite condition for ionization. Therefore, post-column addition of organic solvents (e.g. methanol) and ionization reagents (e.g. chloroform) are normally used for enhancement of ionization efficiency of carbohydrates [1, 2]. However, chloroform may cause strong ion suppression and contamination to the interface and ion optics of LC/MS system. A reduced amount of chloroform in the post-column addition line was used and evaluated in this study.
View here (406800 KB)

LCMS-8040 Application - Highly Sensitive Quantitative Analysis of Amoxicillin and Clavulanic Acid from Plasma Using LC/MS/MS (India)
LC/MS/MS has been increasingly employed in pharmacokinetic studies due to its specificity and sensitivity. This also allows the development of assays with minimal sample preparation. LC/MS/MS method has been developed for highly sensitive quantitation of these molecules from plasma using LCMS-8040, a triple quadrupole mass spectrometer from Shimadzu Corporation, Japan. Ultra fast polarity switching of LCMS-8040 enabled simultaneous analysis of amoxicillin (in positive mode) and clavulanic acid (in negative mode) even in absence of chromatographic separation. Both these molecules were quantitated at low levels with good repeatability even in presence of complex matrix like plasma.
View here (384133 KB)

LCMS-8050 Application - Highly Polar Pesticide Multi-Residue Analysis in Food Safety by LC-MS/MS (UK)
Pesticide residue monitoring laboratories utilise multi-residue LC-MS/MS methods for the quantification of an ever increasing list of target pesticides. However, the measurement of highly polar pesticides by a single LC-MS/MS method is extremely challenging as a consequence of diverse separation and detection behaviour. For this reason, single residue methods or small group specific methods are often utilised to analyse these compounds, in some cases including the use of pre- or postcolumn derivatisation. Therefore, there is a clear need to reduce the number of separation methods applied to the analysis of highly polar pesticides to help accelerate sample throughput, reduce the cost platform, simplify analytical workflows and enhance data quality for regulatory reporting limits.
View here (292178 KB)

Aflatoxins Analysis in Peanut Butter using QuEChERS Sample Preparation with LC‐MS/MS Analysis
Aflatoxins are metabolites produced by fungi (Aspergillus flavus and Aspergillus parasiticus) in high humidity environment in crops such as maize nuts and processed food. Aflatoxin contamination in food is monitored with strict regulations worldwide due to high toxicity of the compounds. Recently, several media reports revealed the exceed levels of aflatoxins found in peanut butters in the USA and Taiwan. Aflatoxins in food have been analyzed by LC/MS/MS using various sample pre-treatment methods. We describe a high sensitivity LC/MS/MS method for quantitative analysis of aflatoxins in peanut butters using QuEChERS sample pre-treatment procedure, as opposed to the use of immunoaffinity column or other methods for sample pre‐treatment which are more expensive and tedious. High sensitivity and good recoveries were achieved using this LC/MS/MS method.
View here (726587 KB)

LCMS-8040 Application - Pesticides in Cannabis
An LC-MS method for detection of pesticides in cannabis with QuEChERS extraction was developed.
View here (1330983 KB)

LCMS-8060 Application - Quantitative Analysis of Residual Artificial Sweetners in Surface Water by Highly Sensitive LC/MS/MS Method (Japan)
Artificial sweeteners are found in surface waters and wastewaters at levels from ng/L to µg/L, which are classified as new emerging environmental contaminants. The artificial sweeteners which have been studied most in this field are acesulfame (ACE), cyclamate (CYC), saccharin (SAC) and sucralose (SUC). LC/MS/MS techniques have been used in these studies. However, pre-concentration of water sample is often required because of the needs for detection of trace levels of the compounds. A LC/MS/MS method was developed previously on LCMS-8040 for identification and quantification of ten artificial sweeteners in beverages. In this Application News, a new LC/MS/MS method on LCMS-8060 is described, aiming at achieving ultra high sensitivity for direct quantitation of above-mentioned five artificial sweeteners in surface waters and drinking waters.
View here (467638 KB)

MALDI-Performance Application - Identification of Proteins by LC-MALDI System (2) [Analysis of Carbonylated Proteins] (Japan)
It is suggested that selective neuronal cell death occurs in the hippocampus CA1 area due to transient cerebral ischemia, resulting in memory impairment. Here, using a sample consisting of the hippocampus CA1 area affected by transient cerebral ischemia, twodimensional electrophoresis was conducted, and spots thought to be carbonylated proteins were excised and analyzed by LC-MALDI. The results confirmed the carbonylation of the 469th arginine of the Heat shock- 70 kDa protein 1 (Hsp70-1), which plays a role in regulating cell death.
View here (654700 KB)

LCMS-2020 Application - LC/MS Analysis of Perfluorochemicals (PFCs) Using Impurity Delay Method (Japan)
This Application News introduces an example of highspeed analysis of drug degradants by LC/MS. The ultra fast features of the LCMS-2020, scan rates up to 15,000 u/sec and positive/negative polarity switching as fast as 15 msec, were used in combination with in-source CID (Collision Induced Dissociation) to produce experimental results. In addition, formula prediction was conducted using the LCMS-IT-TOF, and separation of the sample components was carried out using the Prominence UFLCXR.
View here (446855 KB)

Melamine Analysis Using Triple Quad LCMS-8030
This fast and reliable LC/MS/MS method for melamine and cyanuric acid is over five times faster than conventional methods for these compounds, with a run time under 60 seconds. The simple sample preparation involves only dilution and a one-step solvent extraction and can be automated for high-throughput sample analysis. The sensitivity is more than adequate to meet regulatory requirements while the speed and reliability enable rapid analysis of large numbers of samples. To access the full issue of LC World talk, please click <a href="http://www2.shimadzu.com/lc_worldtalk/" target="_blank">here</a>.
View here (664910 KB)

[ARCHIVED] Restek Guide Pest.pdf
This technical report describes the first comprehensive 2D LC system, in which the on-line coupling of RP-LC×RP-LC to MS (ITTOF) is investigated. The two dimensions consisted both of a novel fused-core stationary phase specifically designed for peptide separation, interfaced through an electronically activated 2 position, ten-port valve. The performance of the system was assessed by means of tryptic mapping (protein unfolding, trypsin digestion, and reversed-phase chromatography of the peptide samples), followed by ESI MS characterization of α-casein and dephosphorylated α–casein.
View here (4067706 KB)

LCMS-8040 Application - Multiresidue Pesticide Analysis from Dried Chili Powder using LC/MS/MS (India)
We present a novel LC/MS/MS method for quantitative determination of acrylamide in potato chips with using a modi ed QuEChERS procedure for sample extraction and clean-up, achieving high sensitivity and high recovery. A small sample injection volume (1uL) was adopted purposely to reduce the potential contamination of samples to the interface of MS system, so as to enhance the operation stability in a laboratory handling food samples with high matrix contents.
View here (491959 KB)

LCMS-8050 Application - Rapid Development of Analytical Method for Antiepileptic Drugs in Plasma using UHPLC Method Scouting System Coupled to LC/MS/MS (Japan)
Traditionally, pyrethroids are measured by Gas Chromatography with or without mass spectrometry. Here, we report a method using LC-MS/MS to show that LC-MS/MS can measure these compounds traditionally analyzed by GC. This report illustrates a simultaneous analysis of 15 pyrethroids using the Shimadzu UFMS Triple Quadrupole LCMS-8050 with ultrafast polarity switching. The polarity switching speed of the LCMS-8050 is just 5 milliseconds under any conditions.
View here (458557 KB)

LCMS-8050 Application - Quantitative Analysis of Pyrethroids in Soil Using Triple Quadrupole LC-MS/MS (Japan)
Here, an LC/MS/MS method has been developed for high sensitive quantitation of this molecule from plasma using LCMS-8050, a triple quadrupole mass spectrometer from Shimadzu Corporation, Japan. Presence of heated Electro Spray Ionization (ESI) interface in LCMS-8050 ensured good quantitation and repeatability even in the presence of a complex matrix like plasma. Ultra high sensitivity of LCMS-8050 enabled development of a low ppt level quantitation method for Loratadine.
View here (347826 KB)

LCMS-8050 Application - Analysis of Drugs in Putrefied Human Pleural Fluid using Triple Quadrupole LC/MS/MS (Japan)
In this data sheet, tributylamine was used as an ion pair reagent. It illustrates simultaneous analysis of hydrophilic metabolites using a Shimadzu UFMS triple quadrupole mass spectrometer, the LCMS-8040, with a ready-to-use “LC-MS/MS method package for Primary Metabolites”.
View here (306031 KB)

LCMS-8040 Application - Characterization of Products Formed by Forced Degredation of Etodoalc using LC/MS/MS (India)
In this work, acid, base, peroxide, thermal and UV degradation products of Etodolac were studied using a Triple Quadrupole Mass Spectrometer LCMS-8040. Ultra fast scanning and Ultra fast polarity switching of LCMS-8040 enabled higher data points and identification of degradation impurities, present in low concentrations in a single run. Prior to LC/MS/MS analysis, the degradation products were isolated using Shimadzu preparative HPLC.
View here (383539 KB)

LCMS-8050 Application - Low Level Quantitation of Steroids in Milk using LC/MS/MS (India)
A highly specific LC/MS/MS method has been developed for trace level quantitation of steroids in milk using LCMS-8050, a triple quadrupole mass spectrometer from Shimadzu Corporation, Japan. Ultra high sensitivity of LCMS-8050 due to heated ESI source, enabled development of ppt level quantitation for testosterone, progesterone and estradiol.
View here (704387 KB)

LCMS-8050/8060 Application - Lipid Mediator Profiling of Human Serum Using LC/MS/MS (Japan)
Conditions developed for “LC/MS/MS Method Package for Lipid Mediators Ver. 2” which can simultaneously analyze 158 lipid mediator-related compounds, were used as a basis for this application. Note that a single chromatographic analysis is capable of separating a wide range of species such as hydrophilic metabolites tetranor-PGs and hydrophobic arachidonic acid and both positive and negative ions are detected. Method sensitivity was compared between the LCMS-8060 and a conventional LCMS-8050 system. For the LCMS-8-6-, signal intensity was around 3 times higher than that of the LCMS-8050.
View here (1531415 KB)

Quantitative Analysis of Pyrethroids in Soil Using Triple Quadrupole LC-MS/MS
Traditionally, pyrethroids are measured by Gas Chromatography with or without mass spectrometry. Here, we report a method using LC-MS/MS to show that LC-MS/MS can measure these compounds traditionally analyzed by GC. This report illustrates a simultaneous analysis of 15 pyrethroids using the Shimadzu UFMS Triple Quadrupole LCMS-8050 with ultrafast polarity switching. The polarity switching speed of the LCMS-8050 is just 5 milliseconds under any conditions.
View here (340558 KB)

LCMS-8050 Application - LC/MS/MS Method for Quantitative Determination of Ethinyl Estradiol in Human Plasma (Singapore)
An ultra sensitive liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for quantitative analysis of oral contraceptive Ethinyl estradiol (EE) has been developed in human plasma using UHPLC Nexera coupled to LCMS-8040 triple quadrupole mass spectrometer and described here. A two stage sample clean-up and also off-line derivatization using Dansyl chloride enabled ultra sensitivity up to 1.0 pg/mL using 750 µL of human plasma. The method was found to be linear in the range of 1 - 200 pg/mL.
View here (277420 KB)

LCMS-8050 Application - Quantitative Analysis of Steroid Hormones Using Triple Quadrupole LC/MS/MS (Japan)
Steroid hormones are heavily involved with the control of metabolism, neurotransmission, and intracellular signaling, playing critical roles in the proper functioning of the body. Further, not only do steroids play roles in sedation and seizure prevention, they are known to be effective in cancer treatment and regenerative medicine. Steroid quantitation in biological samples is therefor an important tool in clinical research. This Application News introduces the analysis of steroid hormones in human serum by LC/MS/MS following pretreatment using liquid supported ISOLUTE SLE (supported liquid extraction).
View here (1368237 KB)

LCMS-8050 Application - Analysis of Glufosinate, Glyphosate, and AMPA in Drinking Water Using a Triple Quadrupole LC/MS/MS System (Japan)
Glufosinate is a popular amino acid-based herbicide and glyphosate a popular foliage treatment herbicide. Glyphosate metabolizes in soil or water to form aminomethylphosphonic acid (AMPA). In March 2015, Japan’s Ministry of Health, Labour and Welfare, Health Service Bureau, Water Supply Division issued a notification specifying the use of LC/MS/MS for water quality control inspections of glufosinate, since it is one of the pesticides designated for monitoring based on the specified target values for drinking water quality control, but no method for inspecting them has been specified so far.
View here (1064324 KB)

LCMS-8060 Application - High Sensitivity, High-Throughput Quantitiation of Catecholamines and Metabolites in Urine by LC/MS/MS for Clinical Research (Japan)
Catecholamines and their metabolites in circulation are readily excreted to urine, both in free form and in conjugated forms (sulfate or glucoronate), and their levels are higher in urine than in plasma by orders of magnitude. Given this and also the non-invasive nature of sample collection, urinary catecholamines and their metabolites are growing research target in clinical context. Moreover, analysis for such research is increasingly performed by tandem mass spectrometry (LC/MS/MS) since it can selectively detect free and conjugated metabolites at high sensitivity. Our aim in this study is to accelerate clinical research by providing a fast and robust LC/MS/MS method to meet the requirement to quantitate both total (deconjugated by acid hydrolysis) and free catecholamine metabolites.
View here (572101 KB)

LCMS-8060 Application - Development of 2D-LC/MS/MS Bioanalytical Method for Quantitative Determination of Insulin Glargine in Human Plasma (Singapore)
A 2D-LC/MS/MS method has been developed on LCMS-8060 for quantitative analysis of insulin Glargine in human plasma without use of SPE extraction and clean-up. The performance of the method was evaluated thoroughly, including linearity, accuracy, repeatability, recovery, sensitivity and speci city. The LOQ of the method is estimated to be 70 pg/mL in human plasma. The advantages of the 2D-LC/MS/MS method are not only simplifying the sample pre-treatment and enhancing the sensitivity, but also reducing the potential contamination of plasma samples to the interface and lens of MS/MS system.
View here (260433 KB)

LCMS-8040 Application - A combined MRM and SIM Method for Direct Quantitative Determination of Amino Acids in Various Samples on LC/MS/MS (Singapore)
By using the Intrada Amino Acid column, a combined MRM-SIM method has been established for detection and quantification of 20 amino acids in biological and beverage samples. The Intrada Amino Acid column can separate effectively the amino acids without need of pre-column derivatization, which allow direct analysis of amino acids on LC-MS. The advantages of a combined MRM-SIM method on LC/MS/MS are the higher sensitivity for glycine in SIM mode and overall enhanced reliability, robustness and accuracy in comparison with the only MRM method or SIM method.
View here (424492 KB)

LCMS-8060 Application - High Sensitivity, High-Throughput Quantitiation of Catecholamines and Metabolites in Urine by LC/MS/MS for Clinical Research
Catecholamines and their metabolites in circulation are readily excreted to urine, both in free form and in conjugated forms (sulfate or glucoronate), and their levels are higher in urine than in plasma by orders of magnitude. Given this and also the non-invasive nature of sample collection, urinary catecholamines and their metabolites are growing research target in clinical context. Moreover, analysis for such research is increasingly performed by tandem mass spectrometry (LC/MS/MS) since it can selectively detect free and conjugated metabolites at high sensitivity. Our aim in this study is to accelerate clinical research by providing a fast and robust LC/MS/MS method to meet the requirement to quantitate both total (deconjugated by acid hydrolysis) and free catecholamine metabolites.
View here (531568 KB)

LCMS-8045/8050/8060 Application - Analysis of Bromate in Tap Water Using a Triple Quadrupole LC/MS/MS (2 Japan)
Bromate in tap water is generated by advanced water treatment processes such as ozone disinfection in the process of water purification. Potassium bromate has been classified by the IARC (1999) as a Group B2 substance which is possibly carcinogenic to humans, and was added to the water quality standards of Japan in 2004 by the Ministry of Health, Labour and Welfare (MHLW). Upon its addition, ion chromatography postcolumn absorption spectroscopy was designated as the testing method for bromate. In this article, we introduce the results of our examination of LC/MS/MS analysis utilizing a mixed-mode column (multi-mode column) as a new LC separation mode.
View here (220224 KB)

Development of 2D-LC/MS/MS Bioanalytical Method for Quantitative Determination of Insulin Glargine in Human Plasma
Human insulin is an essential factor for regulating the metabolism of carbohydrates. Insulin glargine (Lantus) is one of the recombinant insulin analogues widely-used in diabetic patients to regulate glucose levels. Various bioassays have been used for quantitation of insulin and the analogues in serum/plasma for research and diagnosis. Recently, LC/MS/MS has been applied for quantitative analysis of glargine and other insulin analogues, because it enables to distinguish human insulin and recombinant analogues as well as their metabolites. The American Diabetes Association has recommended the sensitivity of bioassay to achieve an LLOQ of 70 pg/mL [1], which is challenging to the current LC-MS systems. The bioassay reported always require tedious solid phase extraction (SPE) for clean up before injecting into the LC/MS/MS [2, 3]. This motivated this study, aiming at developing a high sensitivity method on the latest LCMS-8060 to determine quantitatively insulin glargine in human plasma with lesser sample preparation steps. We describe a newly developed 2D-LC/MS/MS method for high sensitivity quantitation of insulin glargine spiked in human plasma without SPE clean up.
View here (254125 KB)

High Speed, High Resolution Analysis (Part 41) Carryover Evaluation of Glibenclamide in Human Plasma by Nexera HPLC
LC/MS/MS high-speed, high-resolution analysis methods with columns packed with particles of 2 µm or less are often used for analysis of drugs in human blood plasma. The small particle columns produce dispersion that is even less than that obtained with conventional columns (5 µm particle size), so peaks are taller, thereby enabling quantitation at even higher sensitivity. While this high-sensitivity analysis has become possible, the effect of autosampler carryover on high-sensitivity LC/MS/MS analysis has become a problem. In Application News No. L425, we evaluated the performance of the Nexera SIL-30AC autosampler in the analysis of reserpine in human plasma, and reported its low carryover performance. In addition to the high potential of the SIL-30AC, we believe that rinsing with its powerful and sophisticated multi-solvent configuration was very effective.Here, we report on the effectiveness of the rinse method reported in Application News No. L425, and demonstrate its effectiveness as a rinse method applicable to measurement of a wide range of drugs in plasma.
View here (978221 KB)

Nexera Application - High Speed, High Resolution Analysis (Part 45) Analysis of Pre-Column Derivatized Amino Acids by the Nexera SIL-30AC Autosampler (Part 2)
Previously, in Application News articles L422, L428 and L430, we introduced examples of simultaneous analysis of these 4 substances (b1, b2, G1, and G2) using HPLC and UHPLC. In accordance with the test method specified in the notification of August 16, 2011, after pretreatment using an immunoaffinity column, we conducted quantitation using an HPLC system compliant with the test method, identification using a LC/MS system compliant with the test method, and rapid quantitation and identification using the Nexera USPLC. Here, we present these analyses in addition to the results of the validation.
View here (1048926 KB)

Quantitation by HPLC and Identification by LC/MS for Total Aflatoxins in Food
Aᜀatoxins are mycotoxins that are extremely carcinogenic and acutely toxic. In Japan, foods in which the total aflatoxins (sum of B1, B2, G1 and G2 aflatoxins) are detected at levels exceeding 10 µg/kg are in violation of Article 6, Item 2 of the Food Sanitation Act1).Previously, in Application News articles L422, L428 and L430, we introduced examples of simultaneous analysis of these 4 substances (B1, B2, G1 and G2) using HPLC and UHPLC. In accordance with the test method2) specified in the notification of August 16, 2011, after pretreatment using an immunoaffinity column, we conducted (1) quantitation using an HPLC system compliant with the test method, (2) identification using a LC/MS system compliant with the test method, and (3) rapid quantitation and identification using the Nexera UHPLC. Here, we present these analyses in addition to the results of the validation.
View here (1619969 KB)

LC/MS/MS Analysis of Vitamin D by the Co-Sense for Impurities System
The Co-Sense for Impurities system, as previously described in Application News No. L424, is a complete HPLC configuration that automates the sample pretreatment process in trace level analysis. The earlier article presented an example of high sensitivity detection using analyte extraction and concentration. This system offers analyte concentration and removal of
impurities, and therefore comprises 3 flow lines: one for primary separation, another for concentration, and the third for secondary separation. Since a different mobile Detector B
phase and column can be selected for each flow line, a combination of conditions can be used, including those that are conducive for separation at the primary separation stage and that are appropriate for detection for the secondary separation stage. Here we introduce
an example in which Vitamin D3 capsules were analyzed
by LC/MS/MS using such a method.
View here (961152 KB)

LCMS-8040 Application - Maximizing Efficiency for UHPLC LC-MS/MS Method Development in Clinical Drug Monitoring (Germany)
Pesticides are widely used in agricultural products to protect crops from insect infestation during cultivation and product transport. The abuse of pesticides can cause important environmental pollution in different areas, especially at levels of lakes, rivers and aquifers. For this reason one of the most important and attractive application is the possibility to analyze pesticides in water and better if it is without pretreatment of the sample. Shimadzu in cooperation with Arpa Asti (Italy) developed a system for injection of water samples using a triple quadrupole system using a Solid-Phase Exctraction (SPE) on line. We injected water samples in a LCMS-8030 Shimadzu triple quadrupole instrument coupled Nexera UHPLC instrument in order to identify a mixture of 48 substances.
View here (291375 KB)

Ultra-High Speed Analysis of Ibuprofen by Nexera in Accordance with USP 621
High throughput analys is has been advancing dramatically in recent years with the increasing necessity to improve productivity and operational efficiency. HPLC has also been in the spotlight thanks to significant advances in ultra-high-speed analysis technology, in particular ultra high performance LC and micro-particle column packing material. The recently revised General Chapter 621 of the United States Pharmacopoeia (USP 621) now permits a degree of adjustment of HPLC and GC parameters, specifically aimed at satisfying the requirements of system suitability. Here, using the Nexera ultra high performance liquid chromatograph and the Shim-pack VP-ODS conventional column, in addition to the Kinetex XB-C18 Series Core-Shell fast analysis column, we introduce examples of high-speed analysis of ibuprofen-related substances in conformance with USP 621.
View here (935749 KB)

HPLC Application - Analysis of Organic Acids in Culture Medium Using Post-Column pH Buffering Organic Acid Analysis System
Vitamin D is a fat-soluble vitamin that functions as a hormone in the body to regulate calcium metabolism. In addition, there is a report that vitamin D has a number of other physiological roles, including maintaining muscle strength, modulating immune function, and regulating blood pressure. Moreover, vitamin D functions to help regulate cellular differentiation, the biological process by which cells become specialized for a specific function. Due to these physiological function, vitamin D has been implicated in protection against muscle and weakness, certain autoimmune diseases, hypertension, and even some forms of cancer. This sheet describes analysis of 25 hydroxy vitamin D2 and D3 in human serum using LC/MS/MS with ISOLUTE SLE+
View here (910294 KB)

Method Transfer and High-Speed Analysis of Impurities of Drug by Prominence-i
Here, using the new Prominence-i integrated highperformance liquid chromatograph, we conducted analysis of substances chemically related to bepotastine besilate in accordance with the Japanese Pharmacopoeia, while at the same time comparing the analysis results between those using the Prominence-i (with the standard configuration or with the delay volume-compatible system kit) and those obtained using both the conventional integrated LC-2010 model as well as a third-party company's LC system. In addition, we introduce an example of method transfer from that used with Shimadzu's conventional system or that of a third-party LC system, respectively. At the same time, we introduce an example of high-speed analysis using the Prominence-i (with Low-volume tubing kit installed) in which the analysis time is shortened to about onefourth the time, while conforming to the Japanese Pharmacopoeia default of conditions.
View here (942556 KB)

LCMS-2020 Application - Continuous vs. Segmented Second Dimension System Gradients for Comprehensive Two-dimensional Liquid Chromatography of Sugarcane (Saccharum spp.) (Japan)
Polyphenols in sugarcane (Saccharum spp.) leaf extracts were analyzed by comprehensive two-dimensional liquid chromatography in combination with photodiode array and mass spectrometry (LC×LC-PDA-MS) detection; a micro cyano and a partially porous octadecylsilane column were employed in the rst and the second dimension, respectively. Even using RP mode in both dimensions, a satisfactory degree of orthogonality was achieved by employment of different approaches of gradient elution mode in the second dimension. By means of the investigated set-up, a total of 38 polyphenolic compounds were detected with the complementary data of PDA, MS and an in-house database.
View here (297099 KB)

Nexera UC and GCMS Application - Analysis of Residual Pesticides in Agricultural Products Using Nexera UC Off-line SFE-GC/MS System
Conventionally, analysis of residual pesticides in foods has involved pesticide extraction by a solvent extraction method before analysis by LC/MS or GC/MS. The problem with solvent extraction methods is that sample pretreatment requires a substantial amount of time and effort, and large quantities of organic solvents are used. Supercritical fluid extraction (SFE) that uses supercritical carbon dioxide as the extraction solvent provides good extraction efficiency, where the solvent is similar to gas in terms of low viscosity and high diffusivity, and similar to fluid in terms of high solubility. This allows for extraction within a short period of time. This extraction method is also less damaging to the environment since it uses a smaller amount or organic solvent compared to conventional solvent extraction methods. We introduce an example GC/MS analysis of the pesticides extracted from an agricultural product using the Nexera UC off-line system.
View here (3912818 KB)

LCMS-8030/8040 Application - LC-MS/MS Analysis Using Coinjection Method with SIL-30AC
Sample pretreatment takes time and introduces a potential for human error. For analyses that require sample pretreatment, automation of the pretreatment process is an effective means of improving throughput while maintaining repeatability. Automation also allows for analyses to be performed overnight, which is essential when screening a large number of samples. As well as a powerful rinse mechanism that dramatically reduces carryover, the Nexera Series SIL-30AC autosampler includes a pretreatment function as standard, so large volume samples can be analyzed in succession automatically with no operator intervention. Here we introduce the automation of an internal standard method using this pretreatment function along with the measurement results, for the simultaneous analysis of amino acids and acylcarnitines simultaneous analysis of amino acids and acylcarnitines in a dried blood spot (DBS).
View here (873042 KB)

Nexera Application - Examination of the Sugar Analysis Using HPLC Method Scouting System Coupled to Single Quadupole Mass Spectrometer (Japan)
Pesticides are used widely during cultivation of plants including tobaccos. Although they are not foodstuffs, there has been a global concern in the tobacco industry and public about pesticide residues being taken into the body. LC/MS/MS methods have been employed increasingly in detection and quantification of pesticide residuals in foods and agriculture products. One of the challenges in food safety analysis is the large numbers of pesticides on the watching lists imposed by authorities, which leads to screening analysis using conventional MRM method on triple quadrupole LC/MS/MS to be difficult. The new generation ultra-fast LC/MS/MS technique (>500 MRM transitions per second), which enhances greatly the capacity of MRM method when it is used for screening analysis. Both screening analysis and quantification could be carried out using a single method on the same system. Here we report an example of screening analysis and quantification of pesticides in tobaccos using a ready-to-use Method Package on LCMS-8040 system.
View here (459467 KB)

Nexera-e Application - Analysis of Panax Ginseng by Comprehensive Two-Dimensional Ultra High Performance Liquid Chromatography (Japan)
Comprehensive two-dimensional liquid chromatography (2D-LC) is a powerful tool for the analysis of complex samples including pharmaceutical, biological, and natural products. Recently, UHPLC (Ultra High Performance Liquid Chromatography) has been successfully employed to remarkably decrease analysis time in the second dimension of comprehensive LC, and it is becoming popular to speed up 2D-LC separations. In this study, we employed two-dimensional UHPLC for the analysis of Panax ginseng components, a popular Chinese herbal medicine. A combination of RPLC (low pH) x RPLC (high pH) was selected and the chromatographic behavior of five major ginsenosides (ginsenoside Rg1, Re, Rb1, Rc, and Rd) and other minor compounds was monitored. All experiments have been run on a two-dimensional UHPLC system (Shimadzu Prominence UFLCXR) equipped with four high-pressure pumps, and interfaced through ESI to an hybrid mass spectrometer (Shimadzu LCMS-IT-TOF), which possesses both the MSn ability of an ion trap and the excellent resolution and mass accuracy of time-of-flight. A short column (50 mm length) packed with sub-2mm particles was used as second dimension.
View here (1533787 KB)

LCMS-IT-TOF Application - Determination of Impurities in Pharmaceutical Products by 2D-LC Combined wtih LCMS-IT-TOF Mass Spectrometer (Japan)
Assessment of impurities in finished drug products is one of the most important issues for improving quality. An ion trap (IT) time of flight (TOF) mass spectrometer is a powerful tool for identification of impurities due to the advantages of MSn by an IT and accurate mass analysis by a TOF MS. However, during LC separation, especially for pharmaceutical QC analysis, eluent containing non-volatile salt buffer and ion pair reagent is frequently used, and this is not compatible for ESI-MS. Consequently, there is a methodological consideration for low abundant impurity analyses using a LCMS-IT-TOF. In resolving such a problem, we developed and evaluated an automated online concentration system, which is based on the technique of two dimensional HPLC. The target impurity in the fraction is trapped on the desalting column followed by online loading into a LCMS-IT-TOF MS. In addition, molecular formulation of the target substance with a high degree of reliability can be determined by the accurate mass obtained by an IT-TOF MS.
View here (661517 KB)

Nexera Application - Reducing Organic Acid Analysis Times Using SIL-30AC Autosampler
Organic acid counter-ions found in food and drugs are considered important components as they decide the flavor of food and properties of drugs. Food in particular contains a large number of substances analyzable with LC-MS, though LC-MS is unable to detect formic acid and acetic acid in foods due to its use of formic acid and acetic acid in the mobile phase. Combining ion exclusion mode HPLC with post-column reaction detection (post-column pH-buffered electrical conductivity detection) is an approach that does not use formic acid or acetic acid in the mobile phase, and therefore allows the selective and highly sensitive detection of formic acid-containing and acetic acid containing organic acids. However, this approach uses 2 columns to achieve high resolution separation, which increases time to detection. Another problem with this technique is the large number of constituents targeted by food analysis, and the time required to analyze standard reference solutions for calibration curve creation. This article describes using the overlapping function of SIL-30AC to shorten the time required for continuous analysis of organic acids.
View here (93531 KB)

Performance Comparison of Variable Wavelength and Photodiode Array Detectors
Shimadzu strives to achieve superior detector performance by designing high quality optical benches. To achieve this in both the UV and Vis range, dual lamp detector design is offered for both variable wavelength and PDA models. The SPD-M10A and SPD-M10AV PDA detectors demonstrate comparable UV sensitivity. Both the SPD- M10A and M10AV are approximately one and one-half times higher in sensitivity than the SPD-M6A; and, the SPD- 10AV UV-Vis detector demonstrates six times more sensitivity than its photodiode array counterparts.
View here (184 KB)

Analysis of Ointment
Lotions and ointments are common household items. Ointments are used to relieve itching and inflammation, treat eczema, cure athlete's foot, and for hemorrhoid therapy. Spectrophotometric and acid-base titration methods have been conventionally used to analyze these medicines, but this requires complex sample preparation. Faster identification of active ingredients is achieved using HPLC, with only pretreatment. The analysis of the active ingredients contained in medicines for skin disorders (e.g. impetigo, eczema), analgesic treatments (e.g. arthritis, insect bites, etc.), and anti-fungal medicines (e.g. athlete's foot, ringworm, etc.) are presented in the following chromatograms. Samples were provided be Belbe Chemical Industries, Co. Ltd., Japan.
View here (252 KB)

GPC Analysis of a Non-Ionic Surfactant Mixture
Generally, when analyzing surfactants by GPC, the length of the lipophilic group determines the separation. When surfactant mixtures are analyzed by single-column GPC, the peaks often overlap, creating identification difficulties. This Application Note describes the analysis of surfactants by combining two columns. The Shimadzu Shim-pack GPC column, packed with hydrophobic gel, was used in a series with a Shimadzu Asahipak GS hydrophilic gel column. An injection was made of a mixture of an ester (A), POE (B), and amide (C) type of non-ionic surfactants.
View here (126 KB)

Quantitation of Catechol Estroben in Plasma
Recently, the catechol estrogen in biological samples has received a great deal of attention due to its physiological actions. Radio-immuno Assay (RIA) is currently used as the analysis method. However, 2-hydroxyestrogen is extremely unstable and easily oxidized, and is therefore found only in small amounts. This results in poor sensitivity for analysis by the RIA method. The Shimadzu L-ECD-6A electrochemical detector, however, permits highly sensitive HPLC analysis for catechol estrogen and estrogen compounds.
View here (213 KB)

GPC Analysis of Polymide, Polyamic Acid and 12-Nylon
The GPC analysis of polymers depends upon solvent(s) that can completely dissolve the target polymer. These solvents also serve as the mobile phase in GPC analysis. If an appropriate solvent cannot be found, analyses will not provide accurate molecular weight distribution data. With the development of GPC columns, a variety of solvents (other than the widely used THF and chloroform) can now be used. This greatly increases the type of polymers that can be analyzed by GPC. Examples of the anallysis of polyimide, polyamic acid, and nylon-12 are given below.
View here (273 KB)

Using the Shimadzu HPLC System in the Fuel-Grade Ethanol Production Laboratory
Liquid Chromatography (LC) is any chromatographic procedure in which the moving phase is a liquid. In most cases, a stationary phase is also necessary. High Performance Liquid Chromatography (HPLC) has become the most widely applicable method of chromatographic analysis. Through use of highly efficient column materials (the stationary phase), pumping systems that provide a consistent flow of the mobile phase, and detection components designed to accommodate the needs of the analysis, HPLC is now a commonly used technique for monitoring the progress of the fermentation in the ethanol production laboratory.
View here (879 KB)

Nexera XR Application - High Speed, High Resolution Analysis (Part 26) Analysis of Phenolic Acids
A fine porous polyolefin film is generally used as the separator in a lithium-ion battery, and serves to isolate the anode and cathode while preventing electrons from flowing directly between the anode and cathode, as well as to allow the electrolyte or ions to pass through. Accordingly, these properties are important with respect to the lithium-ion battery’s performance as well as safety. Here we introduce the physical properties test results using both DSC and TMA measurement.
View here (1225991 KB)

Direct LC/MS Analysis of Basic Drugs in Plasma by On-line pretreatment with Weak Cation-Exchange Pretreatment Column
A new pretreatment column, Shim-pack MAYI-WCX (prototype), which has weak cation-exchange groups as stationary phase, has been developed for trapping of basic compounds in consideration of LCMS use. The retention ability and pretreatment effect of the Shim-pack MAYI-WCX was evaluated for desipramine, dibucaine, lidocaine, verapamil and amitriptyline by using a column-switching system (Co-Sense for BA system, Shimadzu).
View here (462368 KB)

High Speed Analysis of Alpha Acids and Iso-Alpha Acids in Beer
In the context of spectrophotometers, the term "detector" refers to a light-receiving element that absorbs the energy of light and consequently induces an electrical change. Types of photoelectric conversion include the external photoelectric effect, a prominent form of which is photoelectric emission from a photoelectric surface into a vacuum, and the internal photoelectric effect, in which photoelectrons are excited into a conduction band. One representative example of a detector based on the former type of photoelectric emission is the photomultiplier tube. Here, of the various aspects of spectrophotometers described in UV Talk Letter Vol. 2, "The Structure of a Spectrophotometer," we will look more closely at these "detectors."
View here (346306 KB)

Prominence Application - High Speed with High Resolution Analysis (Part 29) High Efficiency Analysis of Ferulic Acid in Berry Juice Using Automated Column Switching System
Here we introduce the method of analysis of minerals in dietary supplements as specified in the Pharmacopoeia of the United States (USP 32), where the supplement market now stands at about three trillion yen (33 billion dollars).
View here (241493 KB)

Prominence Application - Applications of Prominence RF-20AXS Fluorescence Detector (Part 3) Analysis of Saccharides Using Post-Column Derivatization System
The Prominence RF-20AXS fluorescence detector not only achieves high sensitivity levels never before seen (water Raman SN ratio greater than 2000), but it also features a temperature-controlled flowcell with a cooling function as standard to provide highly reliable detection unaffected by ambient temperature fluctuations. Here we introduce examples of high sensitivity analysis using the Prominence RF-20AXS.
View here (315761 KB)

Prominence Applications - High-Speed Analysis of Gingerol and Shogaol
In the previous issue, I presented the TGS (pyroelectric) detector, which is included with Shimadzu FTIR spectrophotometers as a standard feature. Another commonly used infrared detector is the MCT detector. In fact, an MCT detector is incorporated in Shimadzu infrared microscopes as a standard feature, and on FTIR spectrophotometers as an option. Because the MCT detector and TGS detector are based on a different detection principle, there are various differences in the characteristics of the two.
View here (339538 KB)

Identification of Proteins by LC-MALDI System (2) - Analysis of Carbonylated Proteins
Using the AXIMA MALDI-TOF-MS system for end-point analysis of two-dimensional electrophoresis, we analyzed carbonylated proteins in the CA1 area of a monkey hippocampus affected by ischemia-reperfusion.It is known that reactive oxygen species, or oxygen radicals (ROS), negatively impact a great many diseases, including cancer, cardiac disease and cerebral stroke, which are the leading causes of death among the Japanese, in addition to such lifestyle diseases as diabetes and arteriosclerosis.
View here (654700 KB)

High Speed with High Resolution Analysis -Analysis of humulones and lupulones in Hops
Hops are one of the basic ingredients in beer and contain -acids (humulones) and β-acids (lupulones). During the brewing process the &Alpha;-acids are converted through isomerization into iso-&Alpha;-acids (isohumulons), which are largely responsible for the bitterness of beer. β-acids, on the other hand, do not produce much bitterness during the boiling stage of beer production, but they are said to play a role in &quot;balancing&quot; the bitter flavor during fermentation and storage. HPLC is generally used for the analysis of &Alpha;-acids and &Beta;-acids, but this analysis typically takes as long as 30 minutes. Here we introduce an example of high-speed analysis of &Alpha;-acids and &Beta;-acids in hops using the Prominence UFLCXR ultra fast, high resolution LC system with a high-speed, high-resolution column.
View here (245027 KB)

High Speed with High Resolution Analysis - High Efficiency Analysis of Ferulic Acid in Berry Juice Using Automated Column Switching System
Here, we introduce an example of analysis of ferulic acid in berry juice using a system constructed specifically for efficient handling of this application. Shimadzu’s Prominence UFLC ultra fast LC system forms the base of the system, which also includes a column switching system comprising the first dimension separation column, a trap column, and the second dimension separation column.
View here (241493 KB)

Applications of the Prominence RF-20AXS Fluorescence Detector - High-Speed Analysis of Tocopherols and Polycyclic Aromatic Hydrocarbons
The Prominence RF-20AXS fluorescence detector not only achieves higher sensitivity than ever before possible (water Raman SN ratio greater than 2000), it also includes as a standard feature a temperature controlled cell with a cooling function to provide highly reliable detection irrespective of ambient temperature fluctuations. Moreover, its excellent performance as a fluorescence detector for ultra fast LC is demonstrated with its high-speed sampling and fast response. Here we introduce examples of high-speed analysis of tocopherols and polycyclic aromatic hydrocarbons using the Prominence RF-20AXS.
View here (310796 KB)

Prominence Application - High Speed Analysis of Tocopherol
This Application News introduces the tensile test and cutting test of Japanese soumen vermicelli to evaluate the texture. Soumen vermicelli is originated in Nara Prefecture in Japan. It was made by hand by kneading wheat, salt, and water; applying food oil and starch; and then stretching, drying, and maturing. Nowadays, it is generally machine-made. According to JAS (Japan Agricultural Standards) standards, noodles less than 1.3 mm diameter are "soumen," those from 1.3 mm to 1.7 mm diameter are "hiyamugi," and larger noodles are classified as "udon."
View here (344303 KB)

Prominence Application - High Speed, High Resolution Analysis (Part 31) Analysis of Mexiletine, Pilsicainide, and Zonisamide in Serum
Phthalate is the generic term for the esters combined phthalic acid and various alcohols that are widely used as a plasticizer for various synthetic resin. Here we present the retention behavior and examples of high-speed analysis of phthalates using the ultrahigh speed Prominence UFLC system and various high-speed, high-resolution Shim-pack XR series columns.
View here (212039 KB)

Prominence Application - High Speed, High Resolution Analysis (Part 32) Analysis of Phthalates Using Shim-pack XR Series Columns
Here we present an example of measurement of a sodium dodecylbenzenesulfonate solution, in addition to measurement of a sample containing less than 0.050 mg/L TOC using the Shimadzu combustion catalytic oxidation type TOC-VCPH total organic carbon analyzer.
View here (305022 KB)

Nexera Application - The Ultimate in Speed and Resolution
In liquid chromatography acetonitrile is often a mobile phase ingredient of choice because of its elution strength in reverse phase analysis, low viscosity, low absorption in a wide range of the UV spectrum, and relatively low cost. However, in order to improve peak selectivity, researchers sometimes need to look for alternative solvents. Due to a wide pressure range of up to 130 MPa Nexera affords unlimited flexibility in choosing the ideal composition of the mobile phase even utilizing such viscous solvents as methanol-water that significantly increase the back pressure.
View here (189825 KB)

Nexera Application - The UHPLC with the Finest Reproducibility under Ultra-High Speed
Nexera supports the use of long analytical columns thereby maximizing separation efficiency thanks to a high pressure limit of up to 130MPa. In this example, two 150 mm columns with 1.8 µm particle size were connected sequentially thereby increasing Nexera’s theoretical plate number to about 70,000.
View here (162134 KB)

Nexera Application - The UHPLC with the Ultimate in Resolution
The Nexera addresses all analysis requirements : conventional / ultra-high speed / ultra-high resolution / high temperature, with no compromise in data integrity. The wide pressure range increased up to 130 MPa allows Nexera to maximize performance of sub-2-micron particles column. The combination of maximized pressure range and high resolution columns such as sub-2 micro columns realizes genuine ultra high speed and ultra high resolution analysis. The following are the examples of analytical data obtained using the Nexera UHPLC. The data demonstrates the ultrahigh speed and ultra-high resolution that can be obtained with this system.
View here (225972 KB)

Nexera Application - The Lowest Near Zero Carryover
Drawing upon innovations developed by Shimadzu across all industries and applications Nexera achieves superb reproducibility of retention time, separation and the peak area through accurate control of the injection volume, temperature, precise solvent delivery and mixing of solvents. The micro plunger-driven precision solvent delivery control can keep up with the demanding flow rate changes required during the rapid concentration shifts in fast gradient programming. Nexera also offers a ultra-low volume mixer ( 20 μL) based on micro reactor technology. The data demonstrates ultra-fast gradient analysis of alkylphenones.
View here (231701 KB)

Nexera Application - Impurity Analysis by High-sensitivity UV Detector
Nexera autosampler has been designed to provide our customers with the next generation tools for combating sample carryover on an entirely new level. It is now possible to perform a thorough rinse of the sample path and the needle surface by multiple different solvents eliminating the traces even of the stickiest of compounds. This is in addition to the flow-through needle design with minimized contact area which by itself significantly reduces carryover and insures highly reproducible analysis of trace compounds.
View here (221079 KB)

Nexera Application - Ultra-High-Speed and Ultra-High-Resolution Analysis of Drug Analogs
Red wine contains many types of polyphenols. One of them, resveratrol, is attracting a great deal of attention as an antioxidant that may have the ability to extend life. A high-resolution column is used to resolve the impurity components for the analysis of resveratrol in red wine. A fluorescence detector is effective from both the sensitivity and selectivity viewpoint. This Application Data Sheet introduces the ultra-high-speed analysis of resveratrol in red wine using Nexera with an RF-20Axs high-sensitivity fluorescence detector.
View here (156135 KB)

Nexera Application - Ultra-High-Speed Analysis of Preservatives in Cosmetics
Quinolone antibacterial agents are widely used in livestock, poultry, and farmed fish to prevent and treat infectious diseases. Many types are available. Such simultaneous analysis of multiple components generally requires a long analysis time. However, the combination of a Shim-pack XR Series fast-analysis column and Nexera can significantly reduce the analysis time required. This Application Data Sheet introduces the ultra-high-speed simultaneous analysis of quinolone antibacterial agents using Nexera with an RF-20Axs high-sensitivity fluorescence detector.
View here (146132 KB)

Nexera Application - Ultra-High-Resolution Analysis of Aromatic Carboxylic Acids
Red wine contains many types of polyphenols. One of them, resveratrol, is attracting a great deal of attention as an antioxidant that may have the ability to extend life. A high-resolution column is used to resolve the impurity components for the analysis of resveratrol in red wine. A fluorescence detector is effective from both the sensitivity and selectivity viewpoint. This Application Data Sheet introduces the ultra-high-speed analysis of resveratrol in red wine using Nexera with an RF-20Axs high-sensitivity fluorescence detector.
View here (160353 KB)

Nexera Application - Ultra-High-Speed Analysis of Quinolone Antibacterial Agents
As analogs in drug products often have similar structures, high resolution is demanded for their analysis. A long, sub- 2 μm column is effective in such cases but this requires a UHPLC system with high pressure tolerance, such as the Shimadzu Nexera (130 MPa pressure tolerance). This Application Data Sheet introduces the ultra-high-speed and ultra-high-resolution analysis of ketoprofen and its analogs.
View here (146495 KB)

Nexera Application - Ultra-High-Speed Analysis of Polyphenols in Wine
Parabens and other preservatives are added to cosmetics to maintain safety and quality. The simultaneous analysis of these preservatives generally takes a long time, due to the many types of preservative used. This Application Data Sheet introduces the ultra-high-speed analysis of preservatives in cosmetics using the high resolution of the Shim-pack XR-ODS III column (1.6 µm particle size) and the high pressure tolerance (130 MPa) of the Nexera.
View here (142921 KB)

Ultra-High-Speed Analysis of Polyphenols in Wine (Japan)
Here we introduce analytical conditions that do not include the use of an ion-pair reagent. Using a multi-mode ion-exchange column, a mobile phase consisting only of an aqueous solution of acetic acid and acetate was used. Aminoglycoside antibiotics, compounds that are typically separated by ion-pair chromatography, consists of several sugars and amino sugars. As these compounds display almost no optical absorption, but are easily ionized due to the amino group, a mass spectrometer is the most useful instrument for detection of these compounds.
View here (142921 KB)

Nexera Application - Ultra-High-Resolution Analysis of Polycyclic Aromatic Hydrocarbons
Plants and processed foods contain a variety of hydroxycinnamic acid derivatives and hydroxybenzoic acid derivatives. A high-resolution column is required for their analysis to achieve mutual resolution and resolution from the impurity components in the sample. Methods using a long, sub-2 µm column are available to achieve high resolution, but they demand a UHPLC system with high pressure tolerance. The Nexera 130 MPa pressure tolerance offers adequate capacity to meet these requirements. This Application Data Sheet introduces the ultra-high-resolution analysis of aromatic carboxylic acids using Shimadzu Nexera with a Shim-pack XR-ODS III column.
View here (176486 KB)

High Speed, High Resolution Analysis (Part 33)
Ginger is not only used as a spice, but has also been used in traditional Chinese herbal medicine since ancient times. Investigation into the efficacy of ginger has been attracting a lot of attention in recent years, and the use of ginger in health foods has seen great increases. Here we introduce an example of the analysis of 6-gingerol and 6-shogaol, constituents of ginger, using the Prominence UFLC ultra fast LC system with the SPD-M20A photodiode array detector.
View here (1448233 KB)

HPLC Application - Application of Evaporative Light Scattering Detector (Part 9) Analysis of Dimethicone (Dimethylpolysiloxane) in Hair Care Products
Here we introduce an analysis of fertilizer we conducted using the Shimadzu ICPE-9000 Multitype Inductively Coupled Plasma Emission Spectrometer. ICP-AES features a wide dynamic range and high sensitivity, in addition to its applicability to simultaneous multi-element analysis. It is an extremely efficient analytical method, especially when there are many target elements present in a wide concentration range, from the principle constituents to trace level substances.
View here (1307869 KB)

Prominence Application - Applications of the Prominence RF-20AXS Fluorescence Detector (Part 8) High Sensitivity Analysis of Pirimicarb, Tetracycline, Oxytetracycline, o-Phenylphenol, and Diphenyl
Here, we introduce band gap determination from Tauc plots obtained from diffuse reflectance spectra of samples consisting of compound semiconductor materials, which in this case were provided by the Wada Laboratory, Faculty of Science and Technology, Ryukoku University. The experiments were also conducted with the cooperation of the Wada Laboratory, Ryukoku University.
View here (1382136 KB)

The Application of UHPLC to Reduce Sample Analyses Times
The use of UHPLC technology has continued to increase in LC applications as a way to reduce sample analysis turnaround times. Maintaining or increasing resolution of faster separations has been made possible with the use of small particle column technology. UHPLC often provides run times of less than one minute with peak widths of less than 200 milliseconds that have created challenges for system performance and detection methods. A variety of applications in pharmaceutical and environmental areas with small particle columns will be presented that will demonstrate the throughput and performance that can be obtained with current UHPLC technology.
View here (3481488 KB)

Nexera Application - Ultrafast Analysis of Aldehydes and Ketones
"Various types of synthetic colorants are used as food additives, and gradient elution is generally used to analyze them. Nexera enables stable, ultrafast gradient elution through accurate solution delivery and the use of a high-efficiency gradient mixer. This document introduces an example of ultrafast analysis performed on 12 tar synthetic colorants using Nexera and a Phenomenex Kinetex C18 column (particle size 2.6 µm, a core‐shell column where a 0.35 µm porous membrane is combined with a 1.9 µm solid core)."
View here (210132 KB)

Nexera Application - Ultrafast Analysis of Synthetic Colorants
Water-soluble vitamins such as thiamine (vitamin B1) and riboflavin (vitamin B2) are generally analyzed by reverse-phase ion-pair chromatography. This document introduces an example of ultrafast analysis performed on water-soluble vitamins by gradient elution using Nexera and a Phenomenex Kinetex C18 column (particle size 2.6 µm, a core-shell column where a 0.35 µm porous membrane is combined with a 1.9 µm solid core).
View here (207509 KB)

Nexera Application - Ultrahigh Separation Analysis of Nucleotides
The high sensitivity and selectivity of fluorescence detectors makes them ideal for use in individual test methods such as for pesticide residues in food based on the Japan’s Positive List System. Here we use the Prominence RF-20Axs fluorescence detector to introduce examples of high sensitivity analysis of pirimicarb, tetracycline, oxytetracycline, o-phenylphenol, and diphenyl as individual test method targets based on the Positive List System.
View here (171160 KB)

The Ultimate in Speed and Resolution
The Nexera addresses all analysis requirements : conventional / ultra-high speed / ultra-high resolution / high temperature, with no compromise in data integrity. The wide pressure range increased up to 130 MPa allows Nexera to maximize performance of sub-2-micron particles column. The combination of maximized pressure range and high resolution columns such as sub-2 micro columns realizes genuine ultra high speed and ultra high resolution analysis. The following are the examples of analytical data obtained using the NexeraUHPLC. The data demonstrates the ultra-high speed and ultra-high resolution that can be obtained with this system.
View here (189646 KB)

The UHPLC with the Finest Reproducibility under Ultra-High Speed
Drawing upon innovations developed by Shimadzu across all industries and applications Nexera achieves superb reproducibility of retention time, separation and the peak area through accurate control of the injection volume, temperature, precise solvent delivery and mixing of solvents. The micro plunger-driven precision solvent delivery control can keep up with the demanding flow rate changes required during the rapid concentration shifts in fast gradient programming. Nexera also offers a ultra-low volume mixer ( 20 μL) based on micro reactor technology. The data demonstrates ultra-fast gradient analysis of alkylphenones.
View here (192997 KB)

Achieving Near Zero Carryover
Nexera autosampler has been designed to provide our customers with the next generation tools for combating sample carryover on an entirely new level. It is now possible to perform a thorough rinse of the sample path and the needle surface by multiple different solvents eliminating the traces even of the stickiest of compounds. This is in addition to the flow-through needle design with minimized contact area which by itself significantly reduces carryover and insures highly reproducible analysis of trace compounds.
View here (247390 KB)

Use of Methanol Solvent for Separation
In liquid chromatography acetonitrile is often a mobile phase ingredient of choice because of its elution strength in reverse phase analysis, low viscosity, low absorption in a wide range of the UV spectrum, and relatively low cost. However, in order to improve peak selectivity, researchers sometimes need to look for alternative solvents. Due to a wide pressure range of up to 130 MPa Nexera affords unlimited flexibility in choosing the ideal composition of the mobile phase even utilizing such viscous solvents as methanol-water that significantly increase the back pressure.
View here (162928 KB)

Ultra-High-Speed Analysis of Preservatives in Cosmetics
Parabens and other preservatives are added to cosmetics to maintain safety and quality. The simultaneous analysis of these preservatives generally takes a long time, due to the many types of preservative used. This Application Data Sheet introduces the ultra-high-speed analysis of preservatives in cosmetics using the high resolution of the Shim-pack XR-ODS III column (1.6 µm particle size) and the high pressure tolerance (130 MPa) of the Nexera.
View here (146132 KB)

Ultra-High-Resolution Analysis of Aromatic Carboxylic Acids
Plants and processed foods contain a variety of hydroxycinnamic acid derivatives and hydroxybenzoic acid derivatives. A high-resolution column is required for their analysis to achieve mutual resolution and resolution from the impurity components in the sample. Methods using a long, sub-2 µm column are available to achieve high resolution, but they demand a UHPLC system with high pressure tolerance. The Nexera 130 MPa pressure tolerance offers adequate capacity to meet these requirements. This Application Data Sheet introduces the ultra-high-resolution analysis of aromatic carboxylic acids using Shimadzu Nexera with a Shim-pack XR-ODS III column.
View here (160353 KB)

Ultra-High-Speed Analysis of Quinolone Antibacterial Agents
Quinolone antibacterial agents are widely used in livestock, poultry, andfarmed fish to prevent and treat infectious diseases. Many types are available. Such simultaneous analysis of multiple components generally requires a long analysis time. However, the combination of a Shim-pack XR Series fast-analysis column and Nexera can significantly reduce the analysistime required. This Application Data Sheet introduces the ultra-high-speed simultaneous analysis of quinolone antibacterial agents using Nexera with an RF-20Axs high-sensitivity fluorescence detector.
View here (146495 KB)

Ultra-High-Speed Analysis of Polyphenolsin Wine
Red wine contains many types of polyphenols. One of them, resveratrol, is attracting a great deal of attention as an antioxidant that may have the ability to extend life. A high-resolution column is used to resolve the impurity components for the analysis of resveratrol in red wine. A fluorescence detector is effective from both thesensitivity and selectivity viewpoint. This Application Data Sheet introduces the ultra-high-speed analysis of resveratrolin red wine using Nexera with an RF-20Axs high-sensitivity fluorescence detector.
View here (142921 KB)

Ultra-High-Resolution Analysis of Polycyclic Aromatic Hydrocarbons
As the analysis of polycyclic aromatic hydrocarbons in the environment demands the highly efficient resolution of multiple components, long sub-2 µm columns or multiple columns are often used. Such cases demand a UHPLC system with a high system pressure tolerance. The 130 MPa pressure tolerance of the Shimadzu Nexera can safely and flexibly accommodate such demands. This Application Data Sheet introduces the ultra-high-resolution simultaneous analysis of polycyclic aromatic hydrocarbons using Nexera with two Phenomenex Kinetex columns.
View here (176486 KB)

Ultrafast Analysis of Synthetic Colorants
Various types of synthetic colorants are used as food additives, and gradient elution is generally used to analyze them. Nexera enables stable, ultrafast gradient elution through accurate solution delivery and the use of a high-efficiency gradient mixer. This document introduces an example of ultrafast analysis performed on 12 tar synthetic colorants using Nexera and a Phenomenex Kinetex C18 column (particle size 2.6 µm, a core-shell column where a 0.35 µm porous membrane is combined with a 1.9 µm solid core).
View here (658259 KB)

Ultrahigh Separation Analysis of Nucleotides
For high‐separation analysis of these components, a long column with a particulate packing material can be used. However, both the UHPLC unit and column need to have a high pressure‐resistance. This document introduces an example of ultrahigh separation analysis performed on nucleotides using Nexera, which is resistant to 130MPa, and a Shim‐pack XR‐ODS III column (particle size 2.2µm), resistant to 100MPa.
View here (171160 KB)

Ultrafast Analysis of Water-Soluble Vitamins
Water‐soluble vitamins such as thiamine (vitamin B1) and riboflavin (vitamin B2) are generally analyzed by reverse‐phase ion‐pair chromatography. This document introduces an example of ultrafastanalysis performed on water‐soluble vitamins by gradient elution using Nexera and a Phenomenex Kinetex C18 column (particle size 2.6µm, a core‐shell column where a 0.35µm porous membrane is combined with a 1.9µm solid core).
View here (184821 KB)

Ultrafast, Ultrahigh-Sensitivity Analysis of Aflatoxins
Aflatoxins are mycotoxins with a carcinogenic property and acute toxicity. They are measured by fluorescence detection HPLC and other instruments in order to prevent contaminationof foods. Among four components (B1, B2, G1, G2) quantitated as the total aflatoxin, sensitivity for B1and G1is generally enhanced by a derivatization process using trifluoroacetic acid. Using the RF‐20Axs High‐Sensitivity Fluorescence Detector enables these components to be directly detected at a high sensitivity without any derivatization process. This document introduces an example of ultrafast, high‐sensitivity analysis performed on aflatoxins using Nexera and the RF‐20Axs
View here (199876 KB)

High Speed, High Resolution Analysis (Part 33)Analysis of Gingerol and Shogaol in Ginger
Ginger is not only used as a spice, but has also been used in traditional Chinese herbal medicine since ancient times. Investigation into the efficacy of ginger has been attracting a lot of attention in recent years, and the use of ginger in health foods has seen great increases. Here we introduce an example of the analysis of 6-gingerol and 6-shogaol, constituents of ginger, using the Prominence UFLC ultra fast LC system with the SPD-M20A photodiode array detector.
View here (1449226 KB)

Nexera Application - High Speed, High Resolution Analysis (Part 35) Analysis of Resveratrol in Wine by the Nexera UHPLC System
Recently, in line with the oil-conservation movement, silica, as a non-petroleum resource, is increasingly used as a tire reinforcement filler. Fillers are typically mixed with rubber compounds used in tires to enhance reinforcement of the tire. Because silica has a hydrophilic silanol group on its surface, when added to the lipophilic elastomer rubber, it readily coheres to the rubber without actually bonding to the rubber molecule. Thus, the processibility and mechanical strength of the rubber compound is degraded, greatly affecting tire performance. For this reason, processing with a silane coupling agent is conducted to avoid this shortcoming.
View here (1515985 KB)

High Speed, High Resolution Analysis (Part 35) Analysis of Resveratrol in Wine by the Nexera UHPLC System
Resveratrol, a type of polyphenol, is a phytoalexin that is synthesized by plants when they are exposed to stress due to disease and pests. In addition to providing antioxidative effects, resveratrol is reported to offer other health benefits including support for increased longevity. For these reasons, this substance is actively being researched, and recently, resveratrol is being added to food products and to cosmetics. Here we introduce an example of ultra fast analysis of resveratrol in red wine using the Nexera ultra high performance liquid chromatograph and the Prominence RF-20Axs high-sensitivity fluorescence detector.
View here (1515985 KB)

Nexera Application - High Speed, High Resolution Analysis (Part 39) Analysis of Aflatoxins in Food by Nexera
The effects of increased signal intensity and improved signal-to-noise ratio (S/N) were investigated by eliminating noise with the installation of an overdrive lens in the GCMS-QP2010 Ultra, and verifying the effectiveness using simulation and experimentation by GC-MS. The results confirmed that S/N improved through application of the optimum voltage on the overdrive lens. In addition, it was verified from the results of analysis of 5 ppb chlorpyrifos-methyl by the full-scan method that high-sensitivity analysis is possible using the GCMS-QP2010 Ultra equipped with this technology.
View here (1506786 KB)

HPLC Application - Improvement of Dye-Sensitized Solar Cell Efficiency Through High Purification of Dye
Here, we introduce two cases of analysis of these 4 aflatoxins (b1, B2, G1, G2), using the Prominence RF-20A XS high-sensitivity fluorescence detector, first by fluorescence detection using trifluoroacetic acid derivatization, and then direct detection without TFA derivatization.
View here (1449206 KB)

Prominence Application - Applications Using "Prominence RF-20AXS" Fluorescence Detector (Part 9) Analysis of Aflatoxin B1, B2, G1 and G2 at High Sensitivity
The OPTIC-4 is a multimode injection system with a thermal desorption function that enables performing thermal desorption by placing an adsorbent in the injection port liner cup. In combination with the new MonoTrap adsorbent, the system enables analyzing aroma components with high sensitivity.
View here (1808532 KB)

Nexera Application - High Speed, High Resolution Analysis (Part 40) Analysis of Aflatoxins in Food by Nexera UHPLC with an Immunoaffinity Column for Sample Preparation
Here, we conducted measurements of commercially available care food based on the test methods specified for reviewing the suitability of foods for people with dysphagia. We then classified the food according to the specific standard based on the obtained hardness, adhesiveness, and cohesiveness.
View here (1200983 KB)

Nexera Application - High Speed, High Resolution Analysis (Part 44) Analysis of Pre-column Derivatized Amino Acids by SIL-30AC Autosampler
Here, we report the results of measurement of the particle size distribution in hair conditioner using the SALD-1701 non particle size analyzer. First, we conducted measurement using the typical method of diluting the sample with water, and transferring it to a batch cell. Next, using a high-concentration sample measurement system the original liquid was measured as is, without dilution. A comparison of these results is presented.
View here (882530 KB)

Nexera Application - Post-Column pH Buffered Elextric Conductivity Detection of Organic Acids with Ultra High-Performance Liquid Chromatography
Here, we introduce an example of the determination of 26 amino acids using a different column size and different mobile phase conditions than were used in L432. The automatic pretreatment feature of the SIL-30AC was utilized for derivatization of the amino acids during analysis, thereby enabling the overall analysis time to be substantially shortened.
View here (1298525 KB)

LCMS-8030/8040 Application - Analysis of Impurities in Active Pharmaceutical Ingredients Using the Co-Sense for Impurities System (Japan)
2,4,6-trichloroanisole (TCA) emitted from wine corks can taint wine and cause an objectionable odor. Due to the low threshold value for sensing the odor, highly sensitive measurements are required for monitoring. Conventionally, TCA was measured using methods such as purge and trap, which is very effective in concentrating samples, or thermal desorption. The HS-20 headspace sampler includes a trap function that is able to concentrate headspace gases. This Data Sheet describes an example of high-sensitivity measurement of TCA in wine using an HS-trap GC/MS system.
View here (1335216 KB)

Nexera Application - High-Speed and High-Sensitivity Analysis of Cefazolin Using SPD-M30A
This Application Data Sheet introduces the application of scan data from simultaneous scan/MRM measurement to the Forensic Toxicological Database, leading to comprehensive screening for medicinal toxicants in a whole blood sample. Please refer to this in conjunction with Application Datasheet No. 74, which introduces an example of the mass separation of cholesterol from triazolam and etizolam in whole blood, utilizing MRM data from simultaneous Scan/MRM analysis.
View here (233161 KB)

Nexera Application - Ultra-Fast, High Sensitivity Analysis of Degradation Products in Valsartan
The newly-designed capillary SR-Cell (Sensitivity and Resolution Cell) has been adopted for the SPD-M30A highsensitivity photodiode array detector in the Nexera SR Ultra High Performance Liquid Chromatograph. By optimizing the cell's optical path length and diameter, both low noise levels and high sensitivity have been achieved. This article introduces the high-speed, high-sensitivity simultaneous analysis of artificial colorings using the Nexera SR UHPLC and a high-sensitivity cell (option).
View here (225888 KB)

Nexera Application - Ultra-Fast, High-Sensitivity Analysis of Artificial Colorings Using the SPD-M30A Photodiode Array Detector
The need for reliable separation and quantification of minute quantities of pharmaceutical impurities suspected of genetic toxicity continues to grow. Using the SPD-M30A high-sensitivity photodiode array detector permits high-sensitivity detection of extremely trace amounts of components. Introduced here is an example of ultra-fast, high-sensitivity simultaneous analysis of valsartan degradation products.
View here (315927 KB)

Nexera Application - High -Speed, High Resolution Analysis of Water-Soluble Vitamins Using SPD-M30A
The Nexera SR is a high-end model within the Nexera X2 series of ultra high performance liquid chromatographs. It features the SPD-M30A high-sensitivity photodiode array detector which incorporates the newly designed capillary SRCell (Sensitivity and Resolution Cell). Optimization of the optical path length and diameter results in both high sensitivity and low noise. Introduced here is an example of high-speed, high-sensitivity simultaneous analysis of water-soluble vitamins using the Nexera SR ultra high performance liquid chromatograph.
View here (234990 KB)

Nexera Application - Ultra High-Sensitivity Analysis of Degradation products in Valsartan Using SPD-M30A Photodiode Array Detector with High-Sensitivity Cell
The Nexera SR is a high-end model within the Nexera X2 series of ultra high performance liquid chromatographs. It features the SPD-M30A high-sensitivity photodiode array detector which incorporates the newly designed capillary SRCell (Sensitivity and Resolution Cell). Optimization of the optical path length and diameter results in both high sensitivity and low noise. Introduced here is an example of high-speed, high-sensitivity simultaneous analysis of water-soluble vitamins using the Nexera SR ultra high performance liquid chromatograph with high-sensitivity cell (option).
View here (252874 KB)

Nexera Application - Ultra-Fast and High-Sensitivity Analysis of Artificial Colorings Using the SPD-M30A Photodiode Array Detector
The need for reliable separation and quantification of minute quantities of pharmaceutical impurities suspected of genetic toxicity continues to grow. Using the SPD-M30A high-sensitivity photodiode array detector permits high-sensitivity detection of extremely trace amounts of components. Introduced here is an example of ultra-fast, high-sensitivity simultaneous analysis of valsartan degradation products.
View here (311927 KB)

Nexera Application - Ultra High sensitivty Analysis of Water-Soluble Vitamins Using SPD-M30A with High-Sensitivity Cell
The Nexera SR is a high-end model within the Nexera X2 series of ultra high performance liquid chromatographs. It features the SPD-M30A high-sensitivity photodiode array detector which incorporates the newly designed capillary SRCell (Sensitivity and Resolution Cell). Optimization of the optical path length and diameter results in both high sensitivity and low noise. Introduced here is an example of high-speed, high-sensitivity simultaneous analysis of water-soluble vitamins using the Nexera SR ultra high performance liquid chromatograph.
View here (245107 KB)

Nexera Application - Effective Method Development Using Online Blending of Buffer Solutions for Mobile Phase Preparation
This Application Data Sheet introduces an example of screening for environmental pollutants other than PCBs and chlorinated pesticides, which are targeted for MRM measurements, by applying Compound Composer Database Software to the scan data acquired in simultaneous scan/MRM measurements. Also introduced is an accurate trace quantitation analysis of PCBs and chlorinated pesticides with the MRM data acquired in simultaneous scan/MRM measurements in Application Data Sheets No. 78 and No. 79.
View here (1089166 KB)

Nexera Application - Detection of Non-Separated Impurities by i-PDeA
Gas chromatography-mass spectrometry (GCMS) is a technique widely used in this sector, however with analysis runs that may take several hours to complete, and with repeat testing often needed, the market is inevitably calling for increased speed from both preparation methods and instrumentation. As regulations tighten, this speed must still be achieved without any loss of sensitivity and without compromising accuracy or reproducibility. Here we explore some of the latest technology enabling analysts to meet these heightened requirements.
View here (1133296 KB)

Ultra Fast Method Scouting − Maximizing Efficiency for Method Development
The traditional process of investigating analytical conditions during method development is often complicated and time-consuming, and only when it becomes possible for anyone, regardless of skill level, to carry out this task easily, quickly, and ideally as an automated procedure, will greater speed and efficiency raise the overall level of analytical operations. This Report introduces the Nexera Method Scouting system, a UHPLC (ultra high performance LC) system for identifying and resolving the limiting factors associated with traditional method development techniques.
View here (737741 KB)

Prominence Application - Analysis of Anionic Surfactants Using the RF-20A Fluorescence Detector
In anionic surfactant analyses based on inspection methods specified by the water quality standards, five components are targeted: alkyl chains with 10 to 14 carbon atoms. Alkyl chains with the same number of carbon atoms come in two structural isomers: straight-chain and branched-chain. These form multiple peaks, which are then separated and detected. Group quantitation treats alkyl chains with the same number of carbon atoms as a single group. In this method, multiple peak area values are summed for quantitation. This article introduces the method’s operating procedures when using the Shimadzu HPLC LabSolutions workstation.
View here (164282 KB)

Prominence Application - Analysis of Anionic Surfactants Utilizing the RF-20A Fluorescence Detector
In the quantitation of anionic surfactants, mixed standard solutions containing various branched chains of C10 to C14 are used to prepare a calibration curve. The anionic surfactants in the test water are then quantitatively determined after concentration. LabSolutions workstation software features a grouping function for performing the quantitation calculation. This grouping function classifies the approximately 20 peaks (groupings: C10 to C14 in the figure) obtained from the analysis of the mixed standard solutions by the number of carbon atoms (C10 to C14). It then sums the area values (area summation) and creates a calibration curve.
View here (904999 KB)

Ultra Fast Method Scouting − Maximizing Efficiency for Method Development
The traditional process of investigating analytical conditions during method development is often complicated and time-consuming, and only when it becomes possible for anyone, regardless of skill level, to carry out this task easily, quickly, and ideally as an automated procedure, will greater speed and efficiency raise the overall level of analytical operations. This Report introduces the Nexera Method Scouting system, a UHPLC (ultra high performance LC) system for identifying and resolving the limiting factors associated with traditional method development techniques.
View here (737741 KB)

Prominence Application - Analysis of Dicyandiamide in Fertilizers
Amino acids and histamine were derivatized via o-phthalaldehyde (OPA) and chloroformic acid 9-fluorenylmethyl (FMOC) using the automatic pretreatment function of the Nexera X2 Ultra High Performance Liquid Chromatograph (UHPLC) system's SIL-30AC autosampler. A simultaneous analysis of primary amines (OPA derivatives) and secondary amines (FMOC derivatives), which differ in detection wavelength, was enabled by the wavelength switching function of the RF-20Axs fluorescence detector.
View here (232576 KB)

Nexera X2 Application - High-Speed Analysis of Amino Acids and Histamine in Fish Sauce via Automated OPA Pre-column Derivatization
This Data Sheet highlights the pH-buffered electroconductivity method offered by the Shimadzu Organic Acid Analysis System to analyze formic acid, together with a refractive index detector for the simultaneous analysis of formaldehyde.
View here (267707 KB)

HPLC Application - Analysis of Orotic Acid in Yogurt
The present work is focused on the development/optimization of a comprehensive two-dimensional gas chromatography method, with dual detection [flame ionization (FID) and mass spectrometric], for the simultaneous identification and quantification of mineral-oil contaminants in a variety of food products. The two main classes of contaminants, namely saturated and aromatic hydrocarbons, were previously fractionated on a manually-packed silver silica solid-phase extraction (SPE) cartridge. The presence of a series of unknown compounds was investigated using the mass spectrometric data, and were tentatively-identified as esterified fatty acids, most probably derived from vegetable oil based ink.
View here (1175708 KB)

Ultra-Fast, High-Sensitivity Analysis of Artificial Colorings Using the SPD-M30A Photodiode Array Detector
The newly-designed capillary SR-Cell (Sensitivity and Resolution Cell) has been adopted for the SPD-M30A high-sensitivity photodiode array detector in the Nexera SR Ultra High Performance Liquid Chromatograph. By optimizing the cell's optical path length and diameter, both low noise levels and high sensitivity have been achieved. This article introduces the high-speed, high-sensitivity simultaneous analysis of artificial colorings using the Nexera SR UHPLC.
View here (315927 KB)

High-Speed, High-Resolution Analysis of Water-Soluble Vitamins Using SPD-M30A
The Nexera SR is a high-end model within the Nexera X2 series of ultra high performance liquid chromatographs. It features the SPD-M30A high-sensitivity photodiode array detector which incorporates the newly designed capillary SR-Cell (Sensitivity and Resolution Cell). Optimization of the optical path length and diameter results in both high sensitivity and low noise. Introduced here is an example of high-speed, high-sensitivity simultaneous analysis of water-soluble vitamins using the Nexera SR ultra high performance liquid chromatograph.
View here (234990 KB)

Ultra High-Sensitivity Analysis of Degradation products in Valsartan Using the SPD-M30A Photodiode Array Detector with High-Sensitivity Cell
The need for reliable separation and quantification of minute quantities of pharmaceutical impurities suspected of genetic toxicity continues to grow. Using the SPD-M30A high-sensitivity photodiode array detector permits high-sensitivity detection of extremely trace amounts of components. Introduced here is an example of ultra-fast, high-sensitivity simultaneous analysis of valsartan degradation products.
View here (252874 KB)

Ultra-Fast and High-Sensitivity Analysis of Artificial Colorings Using the SPD-M30A Photodiode Array Detector
The newly-designed capillary SR-Cell (Sensitivity and Resolution Cell) has been adopted for the SPD-M30A high-sensitivity photodiode array detector in the Nexera SR Ultra High Performance Liquid Chromatograph. By optimizing the cell's optical path length and diameter, both low noise levels and high sensitivity have been achieved. This article introduces the high-speed, high-sensitivity simultaneous analysis of artificial colorings using the Nexera SR UHPLC and a high-sensitivity cell (option).
View here (311927 KB)

Ultra High-Sensitivity Analysis of Water-Soluble Vitamins Using SPD-M30A with High-Sensitivity Cell
The Nexera SR is a high-end model within the Nexera X2 series of ultra high performance liquid chromatographs. It features the SPD-M30A high-sensitivity photodiode array detector which incorporates the newly designed capillary SR-Cell (Sensitivity and Resolution Cell). Optimization of the optical path length and diameter results in both high sensitivity and low noise. Introduced here is an example of high-speed, high-sensitivity simultaneous analysis of water-soluble vitamins using the Nexera SR ultra high performance liquid chromatograph with high-sensitivity cell (option).
View here (245107 KB)

Analysis of Anionic Surfactants Using the RF-20A Fluorescence Detector
In the analysis of anionic surfactants, of which standard values are specified by the water quality standards in the Japanese Water Supply Act, 250 mL of test water is subjected to 250-fold concentration using a solid phase extraction cartridge. The surfactants are then detected with a fluorescence detector after separation utilizing a reversed phase separation column. In this case, a C18 column, which uses the octadecyl silyl group (C18) as the solid phase, was used. Anionic surfactants C10 to C14, which are subject to analysis, include branched chains. Thus, approximately 20 isomers are separated.
View here (164282 KB)

Analysis of Dicyandiamide in Fertilizers
The dicyandiamide contained in calcium cyanamide is used as a type of nitrification suppressant to inhibit ammonia from changing into nitric acid. In accordance with the partial revision to the matters specifying official standards for general fertilizers based on the Fertilizers Regulation Act (The Ministry of Agriculture, Forestry and Fisheries of Japan; Notification No. 1985; dated August 8, 2012), the content of dicyandiamide-nitrogen in calcium cyanamide is to be 20.0 % or less of the total nitrogen content. This article introduces an example of the analysis of dicyandiamide in fertilizer, with reference to the fertilizer test method (2012) under the supervision of the Japan‘s Food and Agricultural Materials Inspection Center (FAMIC).
View here (232576 KB)

Simultaneous Analysis of Formic Acid and Formaldehyde
Artificial photosynthesis uses photocatalytic reactions for water splitting and carbon dioxide reduction to create hydrogen, oxygen, carbon monoxide, and formic acid. Of these reaction products, hydrogen, oxygen, and carbon monoxide escape from the sample solution as gases. However, formic acid remains in the sample together with added components, such as electron donors, and byproducts, such as formaldehyde. To measure the amount of formic acid created, it is necessary to separate it from these components. This Data Sheet highlights the pH-buffered electroconductivity method offered by the Shimadzu Organic Acid Analysis System to analyze formic acid, together with a refractive index detector for the simultaneous analysis of formaldehyde.
View here (182804 KB)

High-Speed Analysis of Amino Acids and Histamine in Fish Sauce via Automated OPA Pre-column Derivatization
Processed foods and fish containing a significant amount of histamine have resulted in several cases of allergic food poisoning. In Japan, no standard values have been set for histamine concentrations in foods. However, the FDA has specified levels of 50 mg/kg max. for foods in general, the EU has specified 100 mg/kg max. for marine products, and the Codex Alimentarius standard specifies 400 mg/kg max. for fish sauce.
View here (267707 KB)

Effect of Column Temperature on Organic Acid Separation
Shimadzu's organic acid analysis system utilizes ion exclusion chromatography to first separate the target components, then introduce a pH buffer solution by the post-column method to adjust the pH to near neutral, and detect the organic acids using a conductivity detector to permit quantitation of the various organic acids detected. To increase the peak capacity for separations with large numbers of components, this system is often equipped with two columns connected in series. Although the temperatures of these columns are usually set to the same value, setting their temperatures to different values permits adjustment of the separation conditions to improve the resolution of closely eluting organic acids. Here we report the results of analysis of a mixture of organic acids using a dual-column, dual-temperature method.
View here (1025895 KB)

Effective Method Development Using Online Blending of Organic Solvents for Mobile Phase Preparation
When investigating the analytical conditions during HPLC method development, selection of the mobile phase greatly influences the separation. In reversedphase analysis, for example, when the retention and peak shape of an analyte vary greatly depending on the organic solvent used, the separation can often be improved by blending together various organic solvents. However, from the analyst's perspective, every organic solvent mixture prepared must be tested in the actual separation a process that requires a great deal of time and effort. Here, we introduce a technique in which multiple organic solvents are blended online to prepare a mobile phase that is suitable for analysis.
View here (1128929 KB)

Effective Method Development Using Online Blending of Buffer Solutions for Mobile Phase Preparation
When investigating analytical conditions during HPLC method development, selection of the mobile phase greatly influences the separation. In particular, when the analyte is an ionic compound, it is especially important that the mobile phase contains a buffer solution of appropriate pH because the analyte retention varies greatly depending on its ionic dissociation equilibrium. From an analyst's perspective, however, the preparation of several mobile phases at various pH values for each analysis in the investigation of the analytical conditions represents a tedious and time-consuming effort. Here, we introduce a technique in which multiple solutions are blended online to control and adjust the pH of mobile phases for use in analysis.
View here (1089166 KB)

Effective Method Development Using Online Blending of Ion-Pair Reagents for Mobile Phase Preparation
When investigating analytical conditions during HPLC method development, selection of the mobile phase is extremely important due to its effect on analyte separation. In ion-pair reversed-phase mode analysis, the column retention strength changes depending on the concentration of the ion-pair reagent that is added. Therefore, the ion-pair reagent concentration is very important when considering the analytical conditions. However, from the analyst's perspective, the preparation of several mobile phases with different concentrations of ion-pair reagent for each analysis in the investigation of the analytical conditions represents a tedious and time-consuming effort. Here, we introduce a technique in which multiple variants of mobile phase containing different concentrations of ion-pair reagent are prepared online for use in analysis.
View here (1110575 KB)

Nexera-e Application - Comprehensive Two-dimensional Liquid Chromatography for Determination of Polyphenols in Red Wines (Japan)
In this technical report, we investigated a comprehensive two dimensional LC system, comprised of a cation exchange microcolumn loaded whith silver ions (150 x 1.0 mm; 5.0 µm) in 1D and a partially porous column (50 x 4.6 mm; 2.7 µm) in the 2D, in combination with an evaporative light scattering detector (ELSD) and IT-TOF mass spectrometer, for the analysis of TAG fraction of a borage oil sample.
View here (1854072 KB)

HPLC Application - Ultra-High Speed Analysis of USP Methods Conforming to Permissible Limits in New USP General Chapter 621
Kakkonto is a mixture of several traditional Chinese medicines. Type of compounds and their contained amount vary due to their origin. Here, we compared 2D contour plots of four kinds of kakkonto obtained by the Nexera-e comprehensive two-dimensional chromatograph detecting at UV 254nm. Multiple peaks were observed on each chromatogram.
View here (877045 KB)

Nexera-e Application - Analysis of Kakkonto by Nexera-e and SPD-M30A Photodiode Array Detector (Part 2)
Here, using the Shimadzu ICPE-9820 multi-type ICP atomic emission spectrometer, we conducted simultaneous analysis of the minerals among the nutritional components of commercially available foods with nutrient function claims. The ICPE-9820 supports observation in both the axial and radial direction, and permits simultaneous analysis of high-concentration to trace-concentration substances.
View here (1129887 KB)

Comprehensive Two-Dimensional Analysis of Polyphenols in Red Wine Using Nexera-e Coupled with SPD-M30A (Japan)
This application note describes tuning conditions for the Shimadzu GCMS-QP2010 SE (Figure 1) developed to meet the BFB relative abundance criteria described in US EPA methods for analysis of VOCs. Results of an extensive evaluation of the instrument stability using the recommended tune conditions, and a description of the various tune parameter settings are included.
View here (947190 KB)

i-Series Application - Analysis of Anionic Surfactants by Prominence-i and RF-20Axs Fluorescence Detector
According to the Ministerial Ordinance on Water Quality standards, an HPLC method using a fluorescence detector has been adopted as the test method for anionic surfactants. Since either the RF-20A or RF-20Axs fluorescence detector can be connected to the new Prominence-I integrated high-performance liquid chromatograph, the combination of integrated operability and high-sensitivity fluorescence detection is possible. Here we present an example of the analysis of five anionic surfactants using the Prominence-I integrated high-performance liquid chromatograph with the RF-20Axs high-sensitivity fluorescence detector.
View here (1183618 KB)

i-Series Application - High Speed with High Resolution Analysis by Nexera-i Analysis of Cepham Antibiotics
Here we introduce an example of analysis of oligosaccharides in Japanese sake using the Nexera-I integrated high-performance liquid chromatograph, which includes a built-in UV detector. The ELSD-LT II evaporative light scattering detector was connected directly to the Nexera-I through an A/D acquisition
View here (1115652 KB)

HPLC Application - Analysis of Oligosaccharides in Japanese Sake Using an Evaporative Light Scattering Detector
In this report, we introduce an example of analysis in which trap-free two-dimensional HPLC was used to detect impurities using non-volatile mobile phase conditions, which were then converted without complication to volatile mobile phase conditions online to complete the analysis using the LCMS-8040 triple quadrupole mass spectrometer.
View here (1009912 KB)

Comprehensive Two-dimensional Liquid Chromatography/ Triple Quadrupole Mass Spectrometry: the Perfect Marriage
This novel system combines the separation capabilities of comprehensive two-dimensional liquid chromatography (LC×LC), and the specificity and sensitivity of triple quadrupole mass detection (MSMS). The hyphenation of the techniques generates a powerful analytical system, capable of extremely high-resolution power, as well as targeted and untargeted analysis, simultaneously. The so-called selected reaction monitoring (SRM) mode in fact enhanced selectivity, reducing sample consumption and the need for tedious clean-up procedures, specifically for beta-carotene quantification in a red chili pepper extract.
View here (765888 KB)

i-Series Application - High-Speed Analysis of Impurities of Pramipexole Dyhydrocholirde by Prominence-i
The new Prominence-I integrated high-performance liquid chromatograph supports connection with the RID-20A differential refractive index detector. IN addition, as the column oven can house up to three 30cm columns used for GPC analysis, applications that require a long column are also supported. Here, we introduce an example of GPC analysis of polystyrene using the Prominence-I GPC system.
View here (945711 KB)

i-Series Application - Simultaneous Determination of Asulam, Thiophanate-Methyl, Siduron, Iprodine by Prominence-i
In Application News No. 467, we introduced an example of analysis of sugars in juice, in which the Prominence-I was connected to a differential refractive index detector. Here, we introduce an example of simultaneous analysis of sugars and sugar alcohols in an energy drink using the Prominence-I and RID-20A.
View here (963616 KB)

i-Series Application - Analysis of Sugars and Sugar Alcohols in Energy Drink by Prominence-i with Differential Refractive Index Detector
This application note describes a GCMS purge-and-trap (P & T) method validation study conducted to evaluate operating conditions for the existing US EPA Method 624 VOC list, using updated technology and advanced GCMS instrumentation. GCMS instrument operating conditions are provided which bring the method in line with capabilities provided by contemporary laboratory equipment. This application note provides calibration results across three different ranges, complete MDL and Precision and Accuracy studies at multiple concentrations, and analysis of an independent laboratory VOC reference standard and real-world samples.
View here (997708 KB)

Nexera-e Application - Improved Analytical Workflow for Phospholipids by Nexera-e and Co-Sense for Impurities
Smart Metabolites Database registers MRM information of 475 metabolites mainly contained in biological samples such as blood, urine and cells. It enables simultaneous measurement of 475 metabolites using MRM mode. This application data sheet presents an analysis of metabolites in standard human plasma using the scan and MRM methods included in the Smart Metabolites Database, as well as a comparison of the results.
View here (1141513 KB)

Continuous vs. segmented second dimension system gradients for comprehensive two-dimensional liquid chromatography of sugarcane (Saccharum spp.)
Polyphenols in sugarcane (Saccharum spp.) leaves extracts were analyzed by comprehensive two-dimensional liquid chromatography in combination with photodiode array and mass spectrometry (LC×LC-PDA-MS) detection; a micro cyano and a partially porous octodecylsilica columns were employed in the first and the second dimension, respectively. Even using RP mode in both dimensions, a satisfactory degree of orthogonality was achieved by employment of different approaches of gradient elution mode in second dimension. By means of the investigated set-up a number of 38 polyphenolic compounds were detected by means of complementary data of PDA, MS and an in-house database.
View here (495654 KB)

Prominence Application - High-Sensitivity Analysis of 2-AB Glycans by RF-20Axs Fluorescence Detector
Glycans, present in antibody-drug product have an effect on their safety and efficacy, therefor requiring that the types and quantities of the glycans present be investigated. Due to the culture conditions, the diversity and heterogeneity of the glycan structures cannot be avoided so their management must be implemented during the production process. In application News No. L452, the analysis of a pyridylamino (PA)-glycan using a fluorescence detector was introduced. Here, the analysis of 2-aminobenzamide-labelled glycan (2-AB glycan) is introduced. As in Application News No. L452, the world’s highest sensitivity fluorescence detector, the RF-20Axs, was used for detection.
View here (1040010 KB)

i-Series Application - Peptide Mapping of Antibody Drugs by Nexera-i
In this analysis, the MGS-2010 gas sampler was used for the introduction of gas into the instrument; the column was connected using the SPLITTER-INJ (P/N: 221-76252-41). The MGS-2010 is a manual gas sampler for the Tracera (GC-2010 Plus). A purge mechanism is included to reduce the leakage of peripheral air into the system. The SPLITTER-INJ refers to a special injection unit that permits split injection of the sample without requiring that it pass through the standard split/splitless injection unit. Using the MGS-2010 for sample gas injection together with the SPLITTER-INJ unit, it is possible to quantitatively analyze trace level air components, including Oxygen (O2), Nitrogen (N2), etc. with high accuracy.
View here (1072645 KB)

i-Series Application - Analysis of Omeprazole by i-Series for USP and JP Methods
This application news introduces an example of analysis of omeprazole in accordance with the Japanese Pharmacopoeia (JP) and the United States Pharmacopeia (USP). Also presented here is an example of analysis that can be completed in a significantly shorter time than that described in the USP General Chapter 621 Chromatography. The Nexera-I integrated UHPLC was used for analysis by the procedure described in the USP. The Nexera-I supports the use of analytical conditions specified for both HPLC and UHPLC. In the case of compliance (HPLC conditions) with the Japanese Pharmacopoeia, we conducted analysis using the Prominence-I integrated HPLC.
View here (940675 KB)

Nexera UC Application - Analysis of Unstable Compounds Using Online SFE-SFC
Supercritical fluids have the characteristics of both gas and liquid; low viscosity, high diffusivity and solubility. In particular, carbon dioxide becomes a supercritical fluid at a relatively modest critical point. Due to its low toxicity, inertness, easy availability, and low cost, supercritical carbon dioxide fluid is used in a wide variety of fields. Analytical applications using it include supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC).
View here (1036243 KB)

Nexera UC Application - Automated Optimization of Chrial Separation Parameters Using Nexera UC Chiral Screening System
Chiral compound separation by HPLC, which generally uses normal phase conditions, offers the potential for high speed, low organic solvent consumption, low cost, and low environmental impact. However, chiral SFC requires selecting a variety of separation parameters, such as columns and modifiers, which can involve large amounts of time and effort. This article describes using the Nexera UC chiral screening system to automatically optimize the large number of separation parameters by switching between up to 12 columns and various mixture ratios of four types of modifiers. This can significantly reduce the effort required.
View here (1613818 KB)

HPLC Application - Analysis of Cyanide Ion and Cyanogen Chloride in Mineral Water by Post-Column Ion Chromatography
On December 22, 2014, the Japan’s Ministry of Health, Labour and Welfare (MHLW) issued partial amendment to the standards for ingredients in milk and milk products and the regulatory standards for food products and food additives and specified the corresponding testing methods. In these standards, the criteria value for cyanogen in mineral water is specified to 0.01 mg/L (combined total of cyanide ions and cyanogen chloride), with post-column ion chromatography specified as the test method. This example describes using the Shimadzu cyanogen analysis system, compliant with the revised standard for the refreshing drink testing methods, to analyze the cyanide ion and cyanogen chloride levels in mineral water.
View here (1055427 KB)

Comprehensive 2D Separation of Carotenoids in Red Chili Pepper by the Nexera-e System
Carotenoids are naturally occurring organic pigments that are divided into two classes, carotenes, consisting only of carbon and hydrogen, and xanthophylls, which contain oxygen. Carotenoids are rich in double bonds, and therefore have received much attention in recent years as antioxidants, which are known for their disease preventive properties, including lifestyle-related diseases. The extensive range of carotenoids found in foods makes it difficult to conduct simultaneous separation and quantitation by conventional HPLC. However, the Nexera-e comprehensive two-dimensional LC is particularly suited for such analyses.
View here (2209156 KB)

Nexera UC Application - Application of Online SFE-SFC-PDA for Cleaning Validation
Cleaning validation is a process step that is extremely important for ensuring high quality and safety at pharmaceutical manufacturing sites. Cloth used for surface wiping, called a swab, is used to wipe a given part of a piece of manufacturing equipment, and analysis of the wiped area of the swab is performed by using high-performance liquid chromatography (HPLC) or a total organic carbon analysis (TOC). Evaluations using HPLC have been increasingly used in recent years because HPLC enables determination of individual compounds.
View here (1417509 KB)

i-Series Application - Analysis of Aflatoxin B1, B2, G1 and g2 in Kakkonto Using Nexera-i and RF-20Axs
This application news introduces an example analysis of the complex crude drug Kakkonto based on the proposed revision to the Japanese Pharmacopoeia 17th edition. The proposed revision explains a method of analyzing aflatoxins using a fluorescent detector after derivatization with trifluoroacetic acid (TFA). This Application News describes an example analysis performed using this method, and another example analysis performed without derivatization but with direct fluorescence detection.
View here (1237924 KB)

Nexera UC Appliccation - Analysis of Vitamin E in a Commercial Supplement by Offline SFE-SFC-PDA
Vitamin E, also called tocopherol is a fat soluble vitamin and an important chemical substance that exhibits an antioxidant effect, particularly in the human body. There are four tocopherols (α, β, γ and δ) that differ based on the number and position of methyl groups. The α-tocopherol exhibits the strongest antioxidant activity, and this is the tocopherol form found in most commercial supplements as vitamin E. Since it is highly fat-soluble, a quick and simple extraction method using supercritical fluid is expected to be applicable. In this article, we introduce a procedure for α-tocopherol pretreatment that uses supercritical fluid extraction (SFE).
View here (1038463 KB)

Nexera UC and LCMS-8060 Application - Application of Nexera UC SFE Pretreatment System for Extracting Persticide Residues from Soil
Supercritical fluid extraction (SFE) provides excellent extraction efficiency using supercritical carbon dioxide as the extraction solvent, which offers the low viscosity and high diffusivity of a gas and the high solubility of a fluid. Consequently, it extracts target substances quickly using smaller quantities of organic solvent than existing solvent extraction methods, making it a more environmentally friendly method as well. This article describes an example of using the Nexera UC SFE pretreatment system to extract residual pesticides from soil.
View here (1537282 KB)

i-Series Application - BioEthanol Analyzer Application News
HPLC is now a commonly used technique for monitoring the progress of fermentation in the bioethanol production laboratory. In the bioethanol production plant, the HPLC system is typically used to profile the carbohydrate, alcohol, and organic acid contents of the fermentation broth. These compounds display almost no ultraviolet absorption, and are therefore typically detected using a differential refractive index detector. This application shows an example of the analysis of fermentation broth by using a refractive index detector (RID-20A) and a LC-2030C LT integrated highperformance liquid chromatograph.
View here (373933 KB)

HPLC Application - Analysis of ions in Drugs (Part 5) Analysis of Organic Acid Counterions by Ion Exchange Chromatography
Application News No. L457 described an example analysis of chloride, formic acid, acetic acid, and trifluoroacetic acid ions present in drugs using ion chromatography. As mentioned above, drugs can contain multiple different counterions and it is sometimes difficult to separate completely the peaks of these ions using ion chromatography. We describe an example analysis that uses ion exclusion chromatography to increase separation selectively for formic acid, acetic acid, fumaric acid, and maleic acid, which are organic acids frequently used for drug counterions.
View here (773906 KB)

Nexera Application - Development of An UHPLC Method of Simultaneous Determination of Thirteen Bisphenols in Milk Samples
An UHPLC method with using a high sensitivity fluorescence detector was developed for fast, well-separation and high sensitivity analysis of thirteen bisphenols, including the most concerned BPA, BPF, BADGE and BFDGE, in milk samples. This new method shows high sensitivity to low µg/L levels, high accuracy and excellent repeatability. The method was applied to spiked milk samples and the results indicated the good feasibility, high sensitivity and reliability in simultaneous determination of thirteen bisphenols in milk samples.
View here (472888 KB)

Nexera-e Application - Comprehensive 2D Separation of Lipid Species in Mussels Using the Nexera-e System Combined with LCMS-IT-TOF Detection
This article presents an example separation of lipids in mussels using the Nexera-e, which is an effective system for the comprehensive separation of a large number of lipid molecules. A semi-micro-scale separation via the HILIC column was used for the first dimension, and an ultra-high-speed reversed-phase separation was used for the second dimension. An ion trap time-of-flight mass spectrometer (LCMS-IT-TOF) was combined with the Nexera-e to perform detection.
View here (1042846 KB)

i-Series Application - Assay of Aflatoxin M1 in Milk Based on Notification Test Methodology, Using Prominence-i and the RF-20Axs Fluorescence Detector
Aflatoxin M (AFM) is a mycotoxin suspected of carcinogenicity in humans that is detected in the milk of mammals that eat food contaminated with aflatoxin B1. The notification "Handling of Aflatoxin M in Milk" issued on July 23, 2015 (Notification No. 0723-[1] of the Department of Food Safety, PFSB, MHLW) sets a regulatory level for AFM in milk of 0.5 µg/kg, and came into force on January 23, 2016.
View here (812461 KB)

i-Series Application - Analysis of Formaldehyde by the Derivatization-HPLC Method in Compliance with Water Quality Standards
Revisions to the ministerial ordinance related to water quality standards were announced on March 30 2016 (Japan's Ministry of Health, Labour and Welfare Ordinance No. 115; enacted April 1 2016), and Ordinance No. 261 was partially revised. The derivatization-high performance liquid chromatography method was added therein as a formaldehyde inspection method. The standard value remains unchanged at 0.08 mg/L max. This article introduces an example of the analysis of formaldehyde in compliance with the derivatization high performance liquid chromatography method (hereinafter the official method), using a Shimadzu Prominence-i high performance liquid chromatograph.
View here (94063 KB)

i-Series Application - Analysis of Low Molecular Weight Soluble Dietary Fiber by Prominence-i
This application news describes an analysis of the amount of low molecular weight soluble dietary fiber by an enzymatic-HPLC method, based on the Food Labeling Standards ̶ Appendix: Methods of analysis of nutritional composition1). The instrument used was a Prominence-i integrated HPLC system installed with an RID-20A differential refractive index detector
View here (69508 KB)

Prominence Application - Analysis of Nitrous Acid and Ammonium Thiocyanate in Fertilizers
Fertilizers with high concentrations of nitrous acid and ammonium thiocyanate have a negative effect on plant growth, therefore maximum content levels (permitted content levels) for toxic substances are prescribed in official specifications for commercial fertilizers according to the Fertilizer Control Law1). An example of simultaneous analysis of the nitrous acid and ammonium thiocyanate content of fertilizer by HPLC is described. Analysis was performed in conformance with the test method that appears in Testing Methods for Fertilizers (5.8.b and 5.9.a, 2016)2), published by the Food and Agricultural Materials Inspection Center (FAMIC).
View here (75130 KB)

Nexera UC Application - Analysis and Evaluation of Chiral Drugs in Biological Samples Using the Nexera UC-MS/MS System (Japan)
As introduced in Application News No. L495, the optimization for chiral separation using supercritical fluid chromatography (SFC) starts from employing column scouting to find the column and mobile phase appropriate to separation. This article introduces an example of the selectivity and sensitivity of drug level monitoring in a biological sample and the evaluation results of the analysis method, as an application to the pharmacokinetics research of chiral separation using SFC/MS/MS, after having selected an appropriate column.
View here (292882 KB)

High Throughput Analysis of Anti-Epileptic Drugs
Epilepsy is a neurological disorder characterized by varying intensity of seizures. The exact cause of epilepsy is unknown, but any kind of trauma to the brain such as head injury, high fever, large doses of drugs and other toxic substances, or interruption of blood flow to the brain can contribute to seizures.
View here (16 KB)

Aromatic Acid Analysis with an Integrated HPLC System
Aromatic acids are derivatives of phenol and have a wide range of practical uses. Compounds such as benzoic acid and p-hydroxybenzoic acid are common preservatives in beverages, snack foods, and cereals. Others including salicylic acid and acetylsalicylic acid show analgesic, anti-inflammatory, and antiseptic properties.
View here (16 KB)

The HPLC Analysis of Underivatized Amino Acids
Because they lack suitable chromophores, the traditional approach to analyzing amino acids by HPLC is either pre- or post-column derivatization and detection by fluorescence. While this approach yields excellent sensitivity, the derivatization process is time consuming and may introduce variability from run to run.
View here (18 KB)

The HPLC Analysis of Carbohydrates
Carbohydrates from simple sugars to oligo- and poly-saccharides represent an HPLC detection challenge in that they are non-chromophoric. Traditional approaches to their detection, RI and UV (195 - 205nm), are problematic due to issues of poor sensitivity, long detector equilibration times and an inability to handle gradient elution.
View here (34 KB)

The Shimadzu ELSD-LT Evaporative Light Scattering Detector
Evaporative Light Scattering (ELS) detection has entered the HPLC detection mainstream in recent years. It is a valuable complement to UV, PDA and MS, but it is also a preferred detector for such applications as carbohydrates, phospholipids, triglycerides and surfactants. The ELSD makes a light scattering measurement of target analytes that have been dried of mobile phase through evaporation.
View here (18 KB)

Evaporative Light Scattering Detection as a Complement to UV for Flavor Profiling Peppers by HPLC
This data supports the use of 280nm UV for determining only the capsaicins as it is highly selective for those constituents. The ELSD-LT offers numerous advantages: better baseline response for the gradient method, and detection of all flavor constituents, both chromophoric and non-chromophoric, in one run.
View here (184 KB)

The HPLC Determination of Salicin and Polyphenolic Glucosides
Extract from the bark of the White or European Willow, salix alba, has been used as folk medicine for many years in treating inflammation, pain and fever. The principle component of the water extract from salix bark is salicin, 2-(hydroxymethyl)phenyl-â-D-glucopyranoside, a human-metabolic precursor to salicylic acid.
View here (94 KB)

Analysis of Polycyclic Aromatic Hydrocarbone with a Multi-Functional Fluorescence Detector
The multi-functional fluorescence detector RF-550, capable of setting or varying the excitation and fluorescence wavelength by the time program is a new tool useful in simultaneous analysis of plural components differing in the detection optimum wavelength.
View here (95 KB)

Using the HPLC System in the Fuel-Grade Ethanol Production Laboratory
High Performance Liquid Chromatography (HPLC) has become the most widely applicable method of chromatographic analysis. Through use of highly efficient column materials (the stationary phase), pumping system that provide a constant flow of the mobile phase, and detection components designed to accommodate the needs of analysis, HPLC is now a commonly used technique for monitoring the progress of the fermentation in the ethanol production laboratory.
View here (879 KB)

A Practical Approach to Conserving Acetonitrile
Shimadzu offers reasonable and practical analytical tools and solutions to the global acetonitrile shortage. The use of small particle columns with smaller column dimensions has become an increasingly popular way to reduce analysis times, and also provides the additional benefit of decreasing mobile phase consumption.
View here (621 KB)

High Speed Analysis of Explosives
A number of high-speed columns that employ the use of sub 2 micron particles have been fairly recently introduced and can be used for high-speed analysis of explosive compounds. Here, a high-speed explosives method was developed on a larger particle size fused core column that will provide a more rugged assay. Isocratic and gradient conditions were developed for a mixture of EPA 8330 explosive standards.
View here (894902 KB)

Fast Analysis of Vitamins in Dietary Supplements Using LCMS
Utilizing an ultra-fast LCMS with high-speed scan capability and high-speed data acquisition to achieve good linearity and repeatability, as well as accurate quantitative analysis of water-soluble vitamins in dietary supplements.
View here (613807 KB)

Identification of Proteins by LC-MALDI System (1) - Analysis of Samples Obtained from Frozen Tissue Sections
We conducted proteome analysis using a two-dimensional gel electrophoresis system and frozen tissue sections obtained by laser microdissection (LMD).Two-dimensional gel electrophoresis is a technique that is recognized for its excellent reproducibility and its ability to quantitate. Therefore, it is still the most widespread analytical method in proteomics.
View here (584577 KB)

Application of Evaporative Light Scattering Detector - Analysis of Terpenoids in Ginkgo Biloba
Ginkgo biloba extract contains flavonoids and terpenoids that have been reported to be effective for improving poor blood circulation in the brain as well as poor peripheral blood vessel circulation. This ginkgo biloba extract is used as a health dietary supplement in Japan and the United States. Here we present an example of analysis of terpenoids in ginkgo biloba extract using the ELSD-LT II evaporative light scattering detector.
View here (272257 KB)

Analysis of Various Vitamins in Multivitamin Tablets
This application news displays the analysis of various vitamins in multivatamin tablets according to the USP proposed techniques for the analysis of dietary supplements.The United States Pharmacopeia (USP) is an official authority that sets standards for all prescription and over–the–counter drugs, dietary supplements and food ingredients that are intended for sale in the United States.
View here (468968 KB)

Analysis of Ethyl α-D-Glucoside in Sake
Japanese sake typically contains ethyl α-D-glucoside (α-EG), a substance believed to promote beautiful skin, and it is now receiving attention for its effectiveness in improving dry skin conditions even when taken in a drink. Here we present an example of analysis of ethyl α-Dglucoside and other saccharides in sake using hydrophilic interaction liquid chromatography (HILIC).
View here (237122 KB)

High Speed, High Resolution Analysis (Part 30) Analysis of Iso-α-Acids and α-Acids in Beer
Here we introduce an example of analysis of iso-α-acids and α-acids using the ultra-high speed, high resolution Prominence UFLCXR system with a high-speed, highresolution column.
View here (226998 KB)

High Speed, High Resolution Analysis (Part 32) Analysis of Phthalates Using Shim-pack XR Series Columns
Phthalate is the generic term for the esters combined phthalic acid and various alcohols that are widely used as a plasticizer for various synthetic resin. Here we present the retention behavior and examples of high-speed analysis of phthalates using the ultrahigh speed Prominence UFLC system and various high-speed, high-resolution Shim-pack XR series columns.
View here (319009 KB)

Ultra High Performance Liquid Chromatography / Mass Spectrometry Using Open Solution Software
The LCMS-2020, with its high scanning speed (up to 15,000 u/sec) and high-speed polarity switching (15 msec polarity switching), demonstrates the performance that satisfies the demands of UHPLC. The powerful user interface of Open Solution makes data review and verification easy, supporting the chemist who wishes to make rapid yet accurate decisions related to his ongoing research.
View here (449355 KB)

Analysis of Flavonoids in Ginkgo Biloba Extract
Ginkgo biloba leaves are said to contain as many as 20 types of flavonoids,and among these are quercetin, kaempferol and isorhamnetin, 3 types that are present in large quantities.Here we introduce an example of the analysis of these 3 favonoids present in ginkgo biloba leaves using the SPD-M20A photodiode array detector.
View here (1188227 KB)

High Sensitivity Analysis of Pirimicarb, Tetracycline, Oxytetracycline, o-Phenylphenol, and Diphenyl
Here we use the Prominence RF-20AXS fluorescence detector to introduce examples of high sensitivity analysis of pirimicarb, tetracycline, oxytetracycline, o-phenylphenol, and diphenyl as individual test method targets based on the Positive List System.
View here (1382136 KB)

Application of Evaporative Light Scattering Detector (Part 9)Analysis of Dimethicone (Dimethylpolysiloxane) in Hair Care Products
Dimethicone (dimethylpolysiloxane), a type of silicone oil, is widely used in hair care products such as conditioners and shampoos as an emollient that effectively utilizes the water repellent property of this substance.Here, we introduce examples of analysis of dimethicone in hair care products using the ELSD-LD II evaporative light scattering detector.
View here (1307869 KB)

Post-column pH Buffered Electric Conductivity Detection of Organic Acids with Ultra High Performance Liquid Chromatography (Japan)
Here, we introduce examples of Pd trace analysis using the graphite furnace atomization method with the organic solvents isopropanol (IPA) and n-methylpyrrolidone (NMP), both strongly compatible with water and easy to use.
View here (297945 KB)

Application of Evaporative Light-Scattering Detector (Part 10) High Speed Analysis of Glucosylceramide
Here, we introduce an example of high-speed analysis of glucosylceramide in a dietary supplement using the ELSD-LTⅡ evaporative light-scattering detector connected to the Nexera UHPLC (Ultra High Performance Liquid Chromatography) System.
View here (1451748 KB)

High Speed, High Resolution Analysis (Part 37)Analysis of Clobazam and Cibenzoline in Serum by the Nexera UHPLC System
Here, we introduce an example of ultra-high-speed analysis of clobazam and cibenzoline in serum using the Nexera UHPLC (Ultra High Performance Liquid Chromatography) system and the Shim-pack XR-ODSⅢ high-speed separation column (particle size: 1.6 μm).
View here (1217291 KB)

High Speed, High Resolution Analysis (Part 38) Analysis of Artificial Colorings with the Nexera UHPLC System
In this issue, we present an example of ultra-high speed analysis using the Nexera UHPLC (Ultra High Performance Chromatography) System together with the Phenomenex Kinetex C18 high-speed, high-resolution analytical column, developed with the goal of achieving even greater analysis speeds.
View here (2157617 KB)

High Speed, High Resolution Analysis (Part 40) Analysis of Nucleobases, Nucleosides, and Nucleotides by the Nexera UHPLC System
Here, using the Nexera UHPLC (Ultra High Performance Liquid Chromatography) System, and the Shim-pack XR-ODSⅢ and Phenomenex Kinetex C18 high-speed, high-resolution columns, we introduce examples of ultra-high-speed analysis and ultra-high-resolution analysis of nucleic acid-related compounds.
View here (1299167 KB)

Applications Using "Prominence RF-20AXS" Fluorescence Detector (Part 9)Analysis of Aflatoxin 1, B2, G1 and G2 at High Sensitivity
Here, we introduce two cases of analysis of these 4 aflatoxins (B1, B2, G1, G2), using the Prominence RF-20AXS high-sensitivity fluorescence detector, first by fluorescence detection using trifluoroacetic acid derivatization, and then direct detection without TFA derivatization.
View here (1808532 KB)

iPad: Increasing the Productivity of HPLC Systems
The advantage of HPLC system controller web server functionality over workstation networking is the sweeping ability to assess multiple systems on the same network. Combining this feature with the swift startup and portability of the iPad provides even more merits as outlined below.
View here (2351967 KB)

HPLC Application - Improvement of Efficiency for the Method Development in the Laboratory
In this study, we confirmed that the SHIMADZU Nexera UHPLC, which contains an auto-pretreatment function, can realize simultaneous determination of pre-column derivatized primary and secondary AAs with satisfactory performance.
View here (987838 KB)

High Speed, High Resolution Analysis (Part 44)Analysis of Pre-Column Derivatized Amino Acids by SIL-30AC Autosampler
Here, using the RF-20Axs Fluorescence detector and the SIL-30AC autosampler with its automated pretreatment functions, we introduce the analysis of amino acids using pre-column derivatization with OPA and FMOC.
View here (882530 KB)

Prominence Application - High Sensitivity Quantitative Analysis of Trace Level Impurities and Active Ingredients with HPLC
This Application Data Sheet shows the results from analyzing HBCDD in polymers under the same analytical conditions as those in Application Data Sheet 47 using the EGA/PY-3030D Multi-Shot Pyrolyzer and GCMS-QP2020 Ultra.
View here (831900 KB)

Study of an Efficient Method Development and Analysis Preparation Process using UHPLC
An actual analytical HPLC workflow requires time and labor in order to optimize analytical conditions. In this presentation, different processes, including automatic solvent blending and method scouting, as well as the Nexera Quaternary System, are presented, with an emphasis on improving the method development procedure.
View here (334334 KB)

Ultra-high Speed Analysis of Ibuprofen within USP <621> Allowed Limits by Nexera Method Scouting
This application note shows an example of Ibuprofen analysis from the USP-NF. This analysis was based on USP <621> and done by using the Nexera Method Scouting System, with a conventional column, Shim-pack VPODS, and a core-shell column, Kinetex XBC18.
View here (605085 KB)

LabSolutions Application - Procedures for Group Quantitation
This article introduces an example of the analysis of melamine and related substances in fertilizers using an HPLC system, with reference to the fertilizer test methods (2012) under the supervision of the Japan‘s Food and Agricultural Materials Inspection Center (FAMIC).
View here (1159011 KB)

Ultra-Fast Impurity Analysis Using a New High Sensitivity UHPLC Detector
Recently, a new high-sensitivity detector was introduced that provides improved UHPLC system performance with new features that improve workplace efficiency. Results presented will demonstrate the increased sensitivity of this detector. In addition, examples of peak deconvolution capabilities and the detector’s extended dynamic range will be presented.
View here (491236 KB)

High Sensitivity Glycan Profiling in Antibody Drugs using UHPLC and Fluorescence Detection
Non-uniformity of glycans due to the instability of culture conditions used for antibody drugs is a concern which requires rigorous management of the production process. While there is currently no glycan test method specified in the U.S. Pharmacopeia, there is wide demand for such an assessment method. This poster introduces an example of UHPLC analysis of antibody drug glycans.
View here (3053796 KB)

Techniques for Reducing the Effects of Sample Solvent on UHPLC Analyses
For HPLC, sample solvents that adequately dissolve target compounds are required. Therefore, sample solvents that contain a high concentration of organic solvent are often used for reversed phase chromatography. However, these solvents sometimes cause peak broadening. This poster presents techniques to reduce the effects of sample solvents. Recent widespread UHPLC analyses are taken as examples.
View here (549809 KB)

Preparative Separation of Active Components from Natural Products using Low-pressure Gradient Preparative HPLC
Natural products contain a variety of active components, and preparative HPLC is used to separate active components from complex mixtures such as natural products. This poster presents the preparative separation of rosemary using the Prominence low-pressure gradient preparative HPLC system.
View here (319546 KB)

SFC/SFE Application - Supercritical Fluid Chromatography
Advances in column technology have led to a renewed interest in supercritical fluid chromatography, which uses a supercritical fluid as its mobile phase. Compared to liquid, supercritical fluids have low viscosities and high diffusivities. In this report, starting from the basic principles of supercritical fluid chromatography, we introduce examples of high-speed, high-resolution analysis and chiral separation.
View here (335499 KB)

Monitoring the Fermentation Progress in Bioethanol Production Using the Prominence-i Integrated HPLC with Differential Refractive Index Detection
This application shows an example of the analysis of fermentation broth by using a refractive index detector (RID-20A) and a LC-2030C LT integrated high-performance liquid chromatograph.
View here (348125 KB)

LCMS-8030/8040 Application - Screening analysis for drugs of abuse by LC-MS/MS enables fast polarity switching MRM triggered product ion scanning on the fly (SSI)
Surfactant chemistry has made a considerable impact on a number of household products including detergents, shampoos and toothpaste. Products are generally classified by the type of each hydrophilic substructure into anionic, cationic, amphoteric and non-ionic surfactants. Either anionic or non-ionic surfactants are typically used as synthetic detergents, however, to better elucidate the potential risk in environmental samples, mainly in agricultural soils and sediments, methods need to take into account a range of surfactant chemistries. Current surfactant monitoring methodologies tend to focus on a specific surfactant. Here, we have developed the simultaneous analysis method for typical anionic, amphoteric and non-ionic surfactant using LC-MS/MS.
View here (306527 KB)

LCMS-8040 Application - Multiresidue Pesticide Analysis in Crude Food Extracts Using AOC-MEPS and LC/MS/MS (Japan)
Alkylphenol ethoxylates (APEs), kinds of non-ion surfactants, are used in the manufacture of textiles as the detergent and the dispersant in industry. The quantity of production of nonylphenol ethoxylates (NPEs), in which the carbon number of an alkyl group is 9, has most as about 80% in all APEs, and most of remaining is octylphenol ethoxylates (OPEs), the carbon number 8. It is known that APEs can break down to alkyl phenol form by biodegradation. On the other hand, it has been becoming an environmental problem that the surfactant contained in wash drainage makes water quality pollute so it is desired to measure these surfactants with sufficient accuracy. Here, we developed the simultaneous analysis method using LC-MS/MS of typical APEs.
View here (211371 KB)

LCMS-8040 Application - Identification of Antibacterial Component from Extract of Garcinia Indica Fruit Rinds Using LC/MS/MS (India)
Veterinary drugs are widely used in breeding of marine products. However, residual veterinary drugs could enter human body and harm to human health. Therefore, those veterinary drugs in marine products have been strictly regulated in the world. In recent years, the China government continues to strengthen supervision and is developing quicker and highly sensitive analytical method. Usually, the qualitative method of LC/MS/MS is based on the ratio of intensities between qualitative ion and quantitative ion. This paper describes ultra high performance liquid chromatography-triple quadrupole mass spectrometry for rapid screening of 68 veterinary drugs which belong to 12 categories.
View here (159508 KB)

LCMS-8040 Application - Rapid Screening Method Covers Common 161 Forensic Drugs by Ultra-High Speed LC/MS/MS with Synchronized Survey Scanning (Japan)
LC/MS/MS has become an essential tool for the routine analysis in the field of forensic toxicology. It allows you to conduct the simultaneous analysis of multiple compounds in a single run which makes it possible to carry out a fast and high throughput analysis. In this study, we report a newly developed rapid screening method covers common 161 forensic drugs in Japan using ultra-high speed triple quadrupole mass spectrometry. This method also incorporates with information of calibration curve for all 161 using two internal standards. The use of synchronized survey scanning (MRM triggered product ion scanning) output both quantitative and qualitative results in a single run.
View here (413480 KB)

LCMS-8040 Application - Quantitative Analysis of Illegal Dyes in Eggs Using LC/MS/MS (India)
A method for pre-treatment and subsequent LC/MS/MS analysis has been developed for highly sensitive quantitation of these dyes from egg using LCMS-8040, a triple quadrupole mass spectrometer from Shimadzu Corporation, Japan. Ultra-fast scanning speed of LCMS-8040 enables simultaneous analysis of four sudan dyes and para red dye. All these dyes were quantitated at low ppb levels with high specificity and good repeatability even in presence of egg matrix. Sudan and para red dyes consists of a group of synthetic industrial dyes like sudan I, II, III and IV etc. The International Agency for Research on Cancer evaluated the safety of sudan I, II, III and IV in 1987 and considered that they were unclassifiable as to their carcinogenicity to humans. Although there is some evidence that sudan dyes may cause cancer in experimental animals and may cause damage to the genes, there is currently inadequate evidence that they cause cancer in humans. as shown in Figure 3.
View here (1148336 KB)

Analysis of 32 Synthetic PDE‐5 Inhibitors Drugs & Analogues Adulterated in Health Supplements by LC-MS/MS
In recent years, synthe-c phosphodiesterase type 5 enzyme (PDE‐5) inhibitors like sildenafil (active component of VIAGRA) were found as adulterant in some health supplements described as plant or herbal products. Only seven synthe-c PDE‐5 inhibitors, namely, sildenafil, tadalafil, vardenafil, avanafil, udenafil, mirodenafil and lodenafil carbonate are approved officially to be used for the treatment of erectile dysfunction (ED) in men. The adulteration is illegal and may be also dangerous for consumers, because not only the above PDE‐5 inhibitors, many newly appeared analogues that are synthesized with minor modification of the parent structures are also found used as adulterants. Analytical techniques like HPLC and LC/MS/MS have been applied for screening and quantitation of PDE‐5 inhibitors and their analogues. We describe here a high sensitivity LC/MS/MS method for detection and quantification of thirty‐two synthetic PDE‐5 inhibitors and analogues spiked in health products.
View here (1036545 KB)

LCMS-8050 Application - High sensitive quantitation method of perfluoroalkyl acids by an automated online solid phase extraction LC/MS/MS (Japan)
Perfluoroalkyl acids(PFAAs) are widely used as the repellents, the surface coatings of paper, cloth and carpet clothes and the surfactants, etc. However, PFAAs do not decompose easily in the natural environment and can bio-accumulate or build up in certain living organisms. PFAAs are now recognized as emerging pollutants of global relevance which has led to efforts to regulate them and prompted the need for PFAAs monitoring and risk assessment in humans. LC/MS/MS is used for the analysis of PFAAs, where a high selectivity analysis is available. As the analysis sensitivity gets very high, peaks is detected by blank sample or from contamination in preparation step and it sometimes has an influence on quantitative value. In this study we developed the analysis method of PFAAs using LC/MS/MS enormous volume loading to achieve sensitizing and full-automatic in On-line SPE.
View here (684079 KB)

LCMS-8060 Application - Metablolomic profiling of beer types by widely-targeted LC/MS measurement (Japan)
Metabolomics analysis in food science plays a key role for quantitative characterization of food quality. Particularly, it is expected that the development of value-added food production will be boosted thanks to the aid of food metabolomics technology. In this experiment, comprehensive analysis for 97 compounds was performed by a LC-MS/MS to classify five types of beer (two lager beers, an ale type beer, a beer-taste alcoholic beverage and a beer-taste non-alcoholic beverage). Targeted compounds in this analysis are amino acids, organic acids and nucleic acid-related compounds which are known to be the components closely relevant to the sweetness, the bitterness and the flavor in the food. The resulting data from LC-MS/MS analysis were evaluated by statistical analysis (PCA and HCA).
View here (943252 KB)

LCMS-8060 Application - Protein biomarker quantitation from human blood and plasma using novel collection technology by LC/MS/MS (UK, France)
The growth and broad adoption of dried blood spots (DBS) has been driven by the simplicity of the technique for collection, storage and transport of the samples. Its simplicity has resulted in its widespread use in predominantly small molecule applications such as therapeutic drug monitoring and toxicology although DBS has been used in HIV for monitoring antiretroviral (ARV) therapy and in mass spectrometry-based proteomics the focus has been on the analysis of haemoglobin. The limitations of DBS relate not only to sample stability, variable haematocrit levels and matrix effects in the LC-MS/MS analysis but also with the presence of erythrocytes (in the case of ARV therapy proviral DNA leads to an overestimation of viral load). Dried plasma spots (DPS) sampling provides an alternative approach to DBS possibly negating the effect of the haematocrit and reducing matrix effects in LC-MS/MS analysis. This paper compares the distribution of proteins in samples collected by DBS and DPS.
View here (560445 KB)

LCMS-8060 Application - Supercritical fluid chromatography/tandem mass spectrometry analysis of hundreds of pesticide residues in food safety (UK)
Analysis of pesticides in food commodities is typically carried out using gas chromatography/mass spectrometry (GC-MS) and liquid chromatography/mass spectrometry (LC-MS). These two techniques provide an effective combination for the analysis of pesticides with a broad range of physiochemical properties. Supercritical fluid chromatography (SFC) provides an alternative separation method which uses compressed carbon dioxide in supercritical state as its primary mobile phase. The lower viscosity and high diffusivity of the mobile phase in SFC provides lower back pressures in comparison to LC therefore allowing higher flow rates to be used. In addition SFC has lower aqueous-organic solvent consumption. The aim of this work was to demonstrate the application of SFC-MS/MS for the analysis of a broad range of pesticides. To do this a method was developed for the analysis of 338 pesticides commonly analysed by LC-MS/MS (and GC-MS/MS).
View here (773950 KB)

Supercritical fl#31;uid chromatography/tandem mass spectrometry analysis of hundreds of pesticide residues in food safety
Analysis of pesticides in food commodities is typically carried out using gas chromatography/mass spectrometry (GC-MS) and liquid chromatography/mass spectrometry (LC-MS). These two techniques provide an effective combination for the analysis of pesticides with a broad range of physiochemical properties. Supercritical fl#31;uid chromatography (SFC) provides an alternative separation method which uses compressed carbon dioxide in supercritical state as its primary mobile phase. The lower viscosity and high diffusivity of the mobile phase in SFC provides lower back pressures in comparison to LC therefore allowing higher #31;ow rates to be used. In addition SFC has lower aqueous-organic solvent consumption. The aim of this work was to demonstrate the application of SFC-MS/MS for the analysis of a broad range of pesticides. To do this a method was developed for the analysis of 338 pesticides commonly analysed by LC-MS/MS (and GC-MS/MS).
View here (756851 KB)

LCMS-8060 Application - Method conversion tool between instruments for MRM transitions in LCMS adopting conversion factor of collision energy voltage
Triple quadrupole liquid chromatograph mass spectrometer (LC-MS/MS) has been used widely for targeted analysis in omics using huge-multiple MRM transitions and it is common that plural-manufacturers’ mass spectrometers are owned and used in one laboratory. In this case, method transfer to one another instrument is often troublesome and difficult to validate their identity. Furthermore, optimal collision energy voltage in MRM transitions of each compound typically depends on the LC-MS/MS manufacturer. In this study, we obtained the conversion factor of collision energy voltage from the correlation between the value of optimal collision energy voltage at one LC-MS/MS manufacture’s instrument and that at another, and developed a tool to convert a method file from one to another using the conversion factor.
View here (609651 KB)

LCMS-8060 Application - Analytical method development for widely targeted perfluoroalkyl acids (PFAAs) and their precursors in plasma using multi-gradient eluent system by LC-MS/MS (Japan)
As perfluoroalkyl acids (PFAAs) had been widely used because of their excellent surfactant. While the product and usage of perfluorooctane sulfonic acid (PFOS), its salts and perfluorooctane sulfonyl uoride (PFOS-F) were restricted by the Stockholm Convention in 2009, many kinds of precursors which cause PFAAs by decomposition keep being used because they are not restricted. LC-MS/MS analysis methods for PFAAs have been developed, where a high selectivity analysis is available, but it was very difficult to implement the simultaneous analysis of PFAAs and their precursors since the wideness of their chemical property in terms of hydrophilic / hydrophobic. This time, we developed the analytical method for widely targeted PFAAs and their precursors in plasma using multi-gradient eluent system by LC-MS/MS.
View here (1136875 KB)

Simultaneous Analysis of Monovalent and Divalent cations realized by new column Shim-Pack IC-C2
This is to show an example of analysis of inorganic anions, and monovalent and divalent inorganic cations in rainwater using the HIC-6A.
View here (60 KB)

Determination of Ions in Desert Sand
This is an example of analysis of desert sand sampled in Sinkiang-Uighur, China, and inorganic anions and cations were determined by the ion chromatograph HIC-6A
View here (47 KB)

Determination of Aluminum Using On-Column Derivatization
The on-column derivatization is a method of adding a derivatization reagent to a mobile phase to incude derivatization reaction in column, and isolating and detecting.
View here (43 KB)

Analysis of Anion in Environmental Water
Shows examples of Shimadzu HPLC Analysis of environmental water by the LC-6A inorganic ion analysis system
View here (149 KB)

Determination of Carbamate Pesticides by APCI LC/MS
Carbamate pesticides have been used in agricultural pest control in the United States since the 1960s, as contact insecticides. Some have previously been used therapeutically as pediculocides and ectoparasiticides for humans and animals, respectively.
View here (738 KB)

Oil Despersants: Dioctylsulfosuccinate, 2-Butoxyethanol, and Dipropylene Glycol t-Butyl Ether
A rapid LC-MS-MS method for detection of oil dispersants in water was developed.
View here (1071252 KB)

Analysis of Haloacetic Acids in Tap Water Using LC/MS/MS [LCMS-8030]
This Application News introduces an example of analysis of the 3 haloacetic acids using the LCMS-8030 triple quadrupole mass spectrometer and is in accordance with this legislative measure.
View here (976402 KB)

Fast LC-MS/MS Screening Method for Antipsychotics
A fast screening method for a group of typical and atypical antipsychotics has been developed which incorporates the acquisition of full scan MS and data dependent product ion spectra to screen for any untargeted analytes.
View here (900517 KB)

TOC Application - TOC - TOC –Determination in drinking water
Here we introduce an example in which Vitamin D3 capsules were analyzed by LC/MS/MS using such a method.
View here (798777 KB)

LCMS-8030/8040 Application - Designer Cannabinoids (SSI)
A rapid, accurate, and reliable LC-MS-MS method was developed for the determination of 21 controlled substances in urine
View here (386203 KB)

LCMS-8030/8040 Application - Mycotoxins (SSI)
A rapid LC-MS-MS method for determination of designer cannabinoids in smokeable herbs was developed.
View here (317801 KB)

LCMS-8040 Application - Measurement of Homocysteine in Plasma with LCMS-8040 (Japan)
In this study, we report the development of a simultaneous analysis technique for trace amounts of pyrethroids by LC/MS/MS.
View here (887536 KB)

LCMS-8050 Application - A Direct LC/MS/MS Method for Quantitative Determination of 25-Hydroxyvitamin D2 and D3 in Human Plasma (Asia Pacific)
Vitamin-D is an essential nutrient for human health. Vitamin-D deficiency has been reported among populations, which is potentially a factor to develop chronic diseases. The level of vitamin-D is maintained by its metabolite 25OH-vitamin-D2/D3 in the bloodstream. Vitamin-D deficiency is normally defined as its serum level below 50~75nmol/mL. Therefore, accurate measurement of vitamin D status is required in clinical screening test. In recent year, LC/MS/MS has been used for quantitative analysis of vitamin-D metabolites. However, tedious sample preparation is often required such as extraction, derivatization and clean-up with SPE or immunoaffinity columns. This is to remove matrix interferences and increase sensitivity due to poor ionization of the compounds. Furthermore, the amount of serum/plasma required was rather high at 0.5~2 mL per analysis, which is not favourable in the clinical applications. Here, we present a direct high sensitivity LC/MS/MS method for quantitative determination of 25OH-vitamin-D2/D3 in plasma, achieving LLOQ of 3ng/mL with 10uL injection. The method exhibits good accuracy, reproducibility, linearity and specficity over the concentration range from 1-100 ng/mL.
View here (260227 KB)

High-Speed Quantitative Analysis of Antiepileptic Drugs Using Triple Quadrupole LC/MS/MS
This data sheet illustrates high-speed quantitative analysis of 16 anti-epileptic drugs (AEDs) using the Shimadzu UFMS Triple Quadrupole Mass Spectrometer, LCMS-8050.
View here (321123 KB)

Mapping the Hydrophobic Character of Pathfinder Phases
View here (146 KB)

Controlling Selectivity by Means of Temperature in Reversed Phase Chromatography
View here (144 KB)

LCMS-8030/8040 Application - Screening of Sulfa Drugs Using the LCMS-8030 Triple Quadrupole Mass Spectrometer (Japan)
Japan’s Ministry of Health, Labour and Welfare has designated simultaneous analysis using C18 solid-phase extraction and LC/MS to be the official analytical method for managing targeted pesticides in water (revised on April, 2008). Currently, 31 pesticides are covered. This document describes simultaneous MRM analysis using polarity switching with electrospray ionization (ESI) and LC conditions for 30 of these targeted pesticides (excludes Oxine-Cu). The LCMS-8030 is capable of setting the MRM measurement time of each compound independently. In addition, the polarity switching time is short (15msec), making the LCMS- 8030 suitable for simultaneous analysis of multiple compounds that ionize in both positive and negative modes.
View here (335635 KB)

How Hazardous is your Shampoo?
View here (264 KB)

MALDI-Performance Application - Identification of Proteins by LC-MALDI System (1) [Analysis of Samples Obtained from Frozen Tissue Sections] (Japan)
Here, we report on the transmittance measurement of a glass plate coated with TCO film. TCO films are transparent as well as electrically conductive, and examination of the transmittance distribution is important for evaluating both the TCO film and glass substrate. Here we introduce the measurement of the transmittance distribution (map) in glass plate coated with TCO film using the SolidSpec-3700 UV-VIS-NIR spectrophotometer.
View here (584577 KB)

Analysis of Drug Degradants by LC/MS
This Application News introduces an example of highspeed analysis of drug degradants by LC/MS. The ultra fast features of the LCMS-2020, scan rates up to 15,000 u/sec and positive/negative polarity switching as fast as 15 msec, were used in combination with in-source CID (Collision Induced Dissociation) to produce experimental results. In addition, formula prediction was conducted using the LCMS-IT-TOF, and separation of the sample components was carried out using the Prominence UFLCXR.
View here (272103 KB)

LCMS-8030/8040 Application - Achieving Ultra High Speed Analysis with LC/MS/MS (SSI)
High sensitive nano particle size analyzer SALD-7101 H uses high output violet laser (wave length 405nm) and special optical system to realize difficult measurements of the following samples. Low concentration sample of very small particles. Sample particles which can absorb light energy such as carbon black.
View here (717183 KB)

Simultaneous measurement of positive-negative Ions of 30 pesticides for water management using the LCMS-8030 triple quad mass spectrometer.
Japan’s Ministry of Health, Labour and Welfare has designated simultaneous analysis using C18 solid-phase extraction and LC/MS to be the official analytical method for managing targeted pesticides in water (revised on April, 2008). Currently, 31 pesticides are covered. This document describes simultaneous MRM analysis using polarity switching with electrospray ionization (ESI) and LC conditions for 30 of these targeted pesticides (excludes Oxine-Cu). The LCMS-8030 is capable of setting the MRM measurement time of each compound independently. In addition, the polarity switching time is short (15msec), making the LCMS- 8030 suitable for simultaneous analysis of multiple compounds that ionize in both positive and negative modes.
View here (1508144 KB)

LCMS-8030/8040 Application - Analysis of Pesticides Using the Triple Quadrupole LC/MS/MS 8030 (Japan)
Antioxidants, ultraviolet absorbers, flame retardants and other polymer additives are indispensable for improving the characteristics and functionality of polymers. Understanding the types and quantities of these additives to be used is extremely important to effectively control the manufacturing process of the polymers. Here is an example of quantitative analysis of 14 types of polymer additives using MRM (Multiple Reaction Monitoring) and the LCMS-8030 triple quadrupole mass spectrometer.
View here (2868664 KB)

LCMS-8030/8040 Application - Analysis of Polymer Additives Using the LCMS-8030 Triple Quadrupole LC/MS/MS (Japan)
Here, using the Shimadzu MALDI imaging system comprised of the CHIP-1000 and AXIMA Performance to elucidate the distribution of regiospecific energy metabolism-related substances, we introduce our latest reported research results in which the ischemic region reported research results in which the ischemic region and its periphery (ischemic penumbtra) are clearly distinguished.
View here (1431769 KB)

LCMS-IT-TOF Application - Improved Drug Impurity ID Efficiency under CMC Using 2-D LC/MS (Japan)
Here, we report the results of detection of the characteristic fragment ion of βAsp and its differentiation from ordinary Asp using TOF post source decay (PSD) analysis with Shimadzu’s original Curved Field Reflection technology.
View here (2658535 KB)

Analysis of Pesticides Using the Triple Quadrupole LC/MS/MS (LCMS-8030)
According to the list of water quality control substances specified by the Ministry of Health,Labour and Welfare (April, 2010 revision), 31 pesticides are now included as items subject to analysis by "Method 18 - Simultaneous Analysis bySolid-PhaseExtraction-Liquid Chromatography/Mass Spectrometry." Here we conducted analysis of a mixture of 30 of these substances, excluding oxine-copper, but with the addition of Shimazine and Tiobencarb, using LC conditions based on the official method. MRM measurement was conducted by ESI (Electrospray Ionization) using positive-negative switching (Fig. 1). A triple quadrupole liquid chromatograph-mass spectrometer offers excellent sensitivity and selectivity in analysis of complex samples. Setting of the optimum parameters for Multiple-Reaction Monitoring (MRM) transitions is important for obtaining this excellent sensitivity and selectivity.
View here (2868664 KB)

LCMS-8030/8040 Application - Qualitative Analysis of Tochu Tea Using a Triple Quadrupole LC/MS/MS [LCMS-8030] (Japan)
Here, we introduce an example of recovery testing with a sodium dodecylbenzenesulfonate solution using the Shimadzu combustion catalytic oxidation model TOC-L CPH and an example of analysis of a sample with a TOC concentration below 0.050 mg/L.
View here (847460 KB)

TOC Application - TOC-L - Measuring Samples per USP <643> Using Shimadzu TOC-LC*H - Short Version
Here, we introduce the quantitative analysis of sludge and sewage waste water using the ICPE-9000 multitype ICP emission spectrometer. The ICPE-9000 is a multitype inductively coupled plasma emission spectrometer that permits both axial and radial observation. Thus, a wide range of analyses are supported, from trace elements like cadmium, to high-concentration elements like iron and zinc, thereby enabling simultaneous analysis of samples having a wide range of element concentrations, including sewage waste water and sludge.
View here (398438 KB)

LCMS-8030/8040 Application - Analysis of Pesticides in Foods Using a Triple Quadrupole LC/MS/MS [LCMS-8030] (Japan)
Here, using the RF-20Axs fluorescence detector and the SIL-30AC autosampler with its automated pretreatment functions, we introduce the analysis of amino acids using pre-column derivatization with OPA and FMOC.
View here (981656 KB)

Analysis of Geniposidic Acid and Chlorogenic Acid in Tochu Tea Using a Triple Quadrupole LC/MS/MS [LCMS-8030]
Tochu tea made using tochu (Eucommia ulmoides) leaves is well known as one of the 缀ve great traditional Chinese medicines. Tochu tea leaves contain abundant amounts of geniposidic acid (an iridoid glucoside) and chlorogenic acid (3-caffeoylquinic acid). Geniposidic acid is known to possess several pharmacological functions, one of which is the ability to reduce blood pressure. LC/MS is widely used for the analysis of these types of polyphenols in plant extracts. Here, we introduce an analysis of geniposidic acid and chlorogenic acid in tochu tea using a triple quadrupole mass spectrometer.
View here (1005460 KB)

LCMS-8030/8040 Application - Identification of the modified amino acid residue in the modified heme protein using LC-MS/MS (Japan)
This method is used to determine volatile organic compounds in a variety of solid waste matrices. This method is applicable to nearly all types of samples, regardless of water content, including various air sampling trapping media, ground and surface water, aqueous sludges, caustic liquors, acid liquors, waste solvents, oily wastes, mousses, tars, fibrous wastes, polymeric emulsions, filter cakes, spent carbons, spent catalysts, soils, and sediments.
View here (457355 KB)

LCMS-8030/8040 Application - High Throughput LC/MS/MS Analysis of Carbendazin in Orange Juice (SSI)
Amino acids are organic compounds having both an amino group (-NH2) and a carboxylic acid group (-COOH) within the same molecule. However, generally, amino acids also contain imino acids that take on a ring structure as a result of hydrogen in the amino group, such as proline or hydroxyproline, being substituted with the side chain in the molecule.
View here (418659 KB)

LCMS-8030/8040 Application - The application of LC-UFMSMS to the analysis of pesticide residues in negative ion ESI (Austrailia)
Buspirone is an anxiolytic psychoactive drug of the azapirone chemical class, and is primarily used to treat generalized anxiety disorder (GAD). Buspirone is a common model compound for xenobiotic metabolism. Here we describe the application of a Spectral Similarity Correlation methodology (‘S Score’) to the analysis of data generated from a human microsomal incubation of Buspirone. Non-targeted data-dependent MSMS data was collected from a human microsomal incubate using a Shimadzu LCMS IT-TOF system. The ‘S scores’ were derived from the correlation of fragment ion and neutral loss species of unknown chromatographic peaks to those of Buspirone. This approach was unbiased and success was not influenced any user interaction.
View here (554929 KB)

Method Development for Trace Level Detection of N-Nitrosamines in Beer by GC-MS/MS
In Forensic Toxicology, LC/MS/MS has become a preferred method for the routine quantitative and qualitative analysis of drugs of abuse. LC/MS/MS allows for the simultaneous analysis of multiple compounds in a single run, thus enabling a fast and high throughput analysis. But a pretreatment is the most critical step in forensic analysis. In this study, we report a developed analytical system using a modified QuEChERS* extraction method for pretreatment in forensic analysis by high-speed triple quadrupole mass spectrometry
View here (172026 KB)

LCMS-8040 Application - Rapid Screening and Semi-Quantitative Analysis for Forensic Drugs in Blood Using Liquid Chromatography Triple Quadrupole Mass Spectrometry (Japan)
In this study, we report the application of an automated clean-up system using the standalone type AOC-MEPS for analysis of pesticides in food by LC/MS/MS. 138 pesticides are selected as target analytes in the European Union Reference Labolatory (EURL) method. Of these 138 compounds, we analyzed 120 pesticides which could be measured by LC/MS in our previous study.
View here (247198 KB)

LCMS-8040 Application - Targeted Screening and Quantification of Pesticide Residuals in Tobaccos by Ultra Fast LC/MS/MS (Asia Pacific)
Microcystins (MCs) are natural toxins produced by certain general cyanobacteria, which has a strong carcinogenic effect. MCs are seriously harmful to the residents, because they couldn’t be degraded and removed. Therefore, the quantity of MCs in drinking-water is regulated by the WHO. This poster employed a ultra high performance liquid chromatography/electrospray ionization tandem mass spectrometry (UHPLC/ESI-MS/MS) method to determinate 10 MCs in drinking-water. The water samples were prepared without any pretreatment before determination. The method is simple, rapid and highly sensitive, which can meet the requirements for the analysis of MCs in drinking-water.
View here (399529 KB)

LCMS-8030 Application - LC-MS/MS for Screening and Quantifying Anti-Cancer Drugs and Metabolites in Waste Water Rejected in Mediterranean Sea (France)
An on-line sample preparation workstation that automates proteolysis, de-salting and reversed phase chromatography for proteomic workflows has been described. Two major benefits of the system as they relate to food analysis are reproducbility and speed. By configuring the system to enable multiplexing, we have successfully shown the ability to digest and analyze 200 samples per day.
View here (332559 KB)

LCMS-8040 Application - Fast and Sensitive Assay of Tobacco Specific Nitrosamines by UHPLC-MS/MS (France)
Here, we present the application of micro flow LC in comparison to conventional flow LC to minimise the challenges associated with the analysis of spice extracts. Lower flow rates can lead to increased sensitivity for concentration-dependent detection techniques such as electrospray ionization (ESI) mass spectrometry; which consequently permits the injection of smaller volumes of complex matrix into the LCMS system. Matrix effects were compared between conventional flow with the standard injection volume and micro flow employing a lower injection volume.
View here (352028 KB)

GCMS-TQ8030 Application - Analysis of Pesticides in Food Matrix Using QuEChERS by Triple Quadrupole GC/MS/MS and LC/MS/MS (Japan)
Helium gas is typically used as a carrier gas for GC-MS. However, in recent years, the insufficient supply of helium gas and its increase in price have caused problems, prompting global efforts to address these problems. The use of hydrogen gas as an alternative carrier gas holds promise for addressing the issue. This data sheet presents the application of hydrogen carrier gas to the simultaneous analysis of a standard sample of 66 pesticides using the GCMS-QP2010 Ultra, which features a Dual Inlet Turbo Molecular Pump.
View here (767102 KB)

LCMS-8050 Application - Simultaneous Analysis for Forensic Drugs in Human Blood and Urine using Ultra-High Speed LC-MS/MS (Japan)
Here, we describe an example analysis for homocysteine performed using an LCMS-8040 high-performance liquid chromatograph-triple quadrupole mass spectrometer and employing an analytical protocol used by them Mass Spectrometry, Clinical Chemistry and Pharmacology Lab of Meyer Children’s Hospital.
View here (1211839 KB)

LCMS-8050 Application - Multi-residue Analysis of Pyrethroids in Soil and Sediment using QuEChERS by LC/MS/MS (Japan)
Bioactive xenobiotic is removed from the body by metabolism, its conjugated form is often excreted in urine. The identification of the urinary conjugate is important for searching bioactive substance from complex material such as food and herbal medicine. However we have developed compound identification technique using versatile compound database, it is difficult to identify the conjugate by using existing approach because the number of records involving conjugates is insufficient in comparison of deconjugated form. Therefore, we developed the compound identification technique using multistage product ion spectrum with high mass accuracy and newly designed analytical tool using versatile compound database.
View here (484660 KB)

MALDI-iDplus Application - Milk and Dairy Product Profiling Using iDplus
The use of LC-MS/MS for this application is relatively recent, due to the low response of these compounds in LC-MS/MS while low limits of quantification need to be reached. Recently, on-line Solid-Phase-Extraction coupled with UHPLC-MS/MS was described, but in our hands it gave rise to significant carry-over after highly concentrated samples. We propose here a highly sensitive UHPLC-MS/MS method with straightforward QuEChERS sample preparation (acronym for Quick, Easy, Cheap, Effective, Rugged and Safe).
View here (1056488 KB)

LCMS-8050 Application - Low Level Quantitation of Loratadine from Plasma using LC/MS/MS (India)
Efforts have been made here to develop high sensitive methods of quantitation for these two drugs using LCMS-8050 system from Shimadzu Corporation, Japan. Presence of heated Electro Spray Ionization (ESI) probe in LCMS-8050 ensured good quantitation and repeatability even in the presence of a complex matrix like plasma. Ultra high sensitivity of LCMS-8050 enabled development quantitation method at low ppt level for both Felodipine and Hydrochlorthiazide.
View here (470278 KB)

LCMS-8040 Application - Development and Validation of Direct Analysis Method for Screening and Quantitation of Amphetamines in Urine by LC/MS/MS (Asia Pacific)
"The objective of this study was to develop an on-line SPE-LC/MS method for analysis of ve amphetamines in urine without sample pre-treatment except dilution with water. The compounds studied include amphetamine (AMPH), methamphetamine (MAMP) and three newly added MDMA, MDA and MDEA by the new SAMHSA guideline. Four potential interferences and PMPA (R) as a control reference were also included to enhance the method reliability in identification of the five targeted amphetamines from those structurally similar analogues which potentially present in forensic samples."
View here (355718 KB)

LCMS-2020 Application - Simultaneous Screening and Quantitation of Amphetamines in Urine by On-Line SPE-LC/MS (Singapore)
Numerous ambient ionization mass spectrometric techniques have been developed for high throughput analysis of various compounds with minimum sample pretreatment. Desorption corona beam ionization (DCBI) is a more recent technique. In DCBI, helium is used as discharge gas and heating of the gas is required for sample desorption. A visible thin corona beam is formed by using hollow needle/ring electrode structure. This feature facilitates localizing sampling areas and obtaining good reproducibility of data. In this study, DCBI was applied for analysis of various samples.
View here (465236 KB)

LCMS-8040 Application - High-Speed, High-Sensitivity Analysis of Drugs in Plasma Using Triple Quadrupole LC/MS/MS (Japan)
Here, we introduce an example of simultaneous measurement of TOC and TN in seawater using the TOC and TN measurement system consisting of the TOC-L CPH total organic carbon analyzer for microalgal biomass measurement and the TNM-L unit for total nitrogen (TN) measurement.
View here (1043080 KB)

LCMS-8050 Application - Analysis of Nivalenol, Deoxynivalenol, 3-Acetyldeoxynivalenol and 15-acetyldeoxynivalenol Using Triple Quadrupole LC/MS/MS (Japan)
In this application, we investigated the analytical conditions for LC/MS that would permit acquisition of mass information and provide high selectivity in order to eliminate the effects of contaminating components. The LCMS-2020 single quadrupole mass spectrometer was used for the analysis. Good quantitative results were obtained, confirming the applicability of this method suing byproduct compound fertilizer as the actual sample.
View here (978861 KB)

LCMS-8050 Application - Analysis of Diarrhetic Shellfish Toxin Using Triple Quadrupole LC/MS/MS (Japan)
In recent years, there has been a trend toward viewing high concentrations of polycyclic aromatic hydrocarbons (PAHs) in foods (particularly smoked products) as a problem. In 2009, the Codex Alimentarius Commission issued standards for reducing the PAH contamination level in smoked and directly dried foods. In addition, Europe, Canada, South Korea, China, and others established food standards for benzo[a]pyrene. This Application Data Sheet describes using a GC-MS/MS system to analyze the PAHs in "katsuobushi" (dried, smoked, and fermented skipjack tuna, which is very popular in Japanese cuisine).
View here (977703 KB)

LCMS-8050 Application - Quantitative Analysis of Vitamin D Metabolite Using Triple Quadrupole LC/MS/MS (Japan)
Peptide mapping by HPLC is one of the important quality assurance tests used for verifying the primary structure of antibody drugs. Typically, following enzymatic digestion of antibodies, separation is conducted using a traditional reversed phase column. Due to the large number of peaks that require separation, the use of small-particle columns and core shell columns for peptide analysis has spread in recent years. In order to compare elution profiles for identity and mutation confirmation, a highly repeatable system is required. The Nexera-I integrated UHPLC is the ideal system for such an analysis. Here, the Nexera-I is used in the analysis of IgG(human immunoglobulin G tryptic digest).
View here (921984 KB)

LCMS-8050 Application - Comprehensive Analysis of Primary & Secondary Metabolites in Citrus Using an Automated Method Changeover UHPLC System Coupled to LC/MS/MS (Japan)
There is a demand for better tasting, healthier and safer food-stuffs which better meet the needs of both industry and the consumer. New technology has been required to monitor and improve the quality of food, metabolomics has become an important tool for food processing, plant breeding and so on. In-food science, comprehensive analysis of primary metabolites through to secondary metabolites is very important. However, there is no application which can analyze them at the same time. In this study, we developed the analytical methods using LC/MS/MS for monitoring the primary and secondary metabolites in foods, focus on the major compound’s categories such as organic acids, amino acids, sugars, carotenoids and flavonoids.
View here (1047046 KB)

LCMS-8060 Application - High Sensitivity Determination of Catecholamines in Plasma Using the LCMS-8060 LC/MS/MS (Japan)
Catecholamines are a family of signaling molecules found in brain, adrenal medulla and other nervous systems. Catecholamines in plasma, namely norepinephrine (NE), epinephrine (EP) and dopamine (DA), are commonly measured in clinical research. Analysis of catecholamines in plasma requires both high sensitivity and high throughput. Presented here is a platform designed to demonstrate the capability to detect catecholamines in plasma, comprising multiplexed plasma sample preparation by Biotage EVOLUTE WCX solid phase extraction followed by high-sensitivity quantitation by LCMS-8060.
View here (943677 KB)

LCMS-8060 Application - Rapid Quantification of Perfluorinated Compounds in Drinking and Surface Water using LC-MS/MS (SSI)
Though nearly ubiquitous, per uorinated compounds can be effectively and quickly measured directly from surface and drinking water using a modi ed con guration of the LCMS-8050. This method can be used for routine monitoring of PFCs in water samples requiring only minimal sample preparation.
View here (2286112 KB)

LCMS-8050/8060 Application - Lipid Mediator Profiling of Human Serum Using LC/MS/MS
Lipid mediator is a generic term for bioactive lipids, which play a role in many biological functions. Recent development of a high sensitivity ultra-fast mass spectrometer enables lower detection limits for lipid mediator species. A comprehensive and highly sensitive application for the analysis of lipid mediators and their metabolites using a t r i p l e quadrupole mass spectrometer LCMS-8060 is presented here. Conditions developed for “LC/MS/MS Method Package for Lipid Mediators Ver. 2”, which can simultaneously analyze 158 lipid mediator-related compounds, were used as a basis for this application.
View here (149654 KB)

Analysis of Illegal Sudan and Para Red Dyes in Eggs by LC‐MS/MS
Generally, egg yolk color is an indication of its nutritional value and freshness. Eggs with yelloworange hue are the most desired ones. Hence, egg producers enhance the color of their products by feeding the egg laying hens with feed containing various synthetic dyes. This can be proved by confirming the presence of illegal dye residues in eggs. A method for pre-treatment and subsequent LC/MS/MS analysis has been developed for highly sensitive quantitation of these dyes from egg using LCMS-8040, a triple quadrupole mass spectrometer from Shimadzu Corporation, Japan.
View here (1380454 KB)

Eliminating Time Consuming SPE in EPA method 539 for Trace Hormones in Drinking Water by LC‐MS/MS
A fast, selective and highly sensitive method has been developed for the measurement of hormones in drinking water. By integrating a direct high volume injection cycle with a fully optimised LC/MS/MS method, the LCMS-8050 delivers precise and accurate detection limits regulated by EPA method 539 and is in accordance with UCMR3.
View here (896545 KB)

Analysis of Steroids in Milk using QuEChERS Sample Preparation with LC‐MS/MS
A highly specific LC/MS/MS method has been developed for trace level quantitation of steroids in milk using LCMS-8050, a triple quadrupole mass spectrometer from Shimadzu Corporation, Japan. Ultra high sensitivity of LCMS-8050 due to heated ESI source, enabled development of ppt level quantitation for testosterone, progesterone and estradiol.
View here (2170546 KB)

LCMS-8050 Application - Development of a Rapid LC-MS/MS Method for Human Serum Lipid Mediator Profiling (Japan)
An LC-MS/MS method package for lipid mediators was developed to simultaneously analyze 158 lipid mediator related compounds by ultra-fast triple quadrupole mass spectrometry. A list of target components is shown to the right. Optimized MRM transitions and retention times are provided for 87 arachidonic acids and metabolites, 18 EPA and its metabolites, 16 DHA and its metabolites, 11 ethanolamides, 23 metabolites of other fatty acids, Azelaoyl-PAF, PAF and Lyso-PAF.
View here (2054048 KB)

LCMS-8060 Application - LC/MS/MS High Sensitivity Bioanalytical Method: Atorvastatin Calcium in Human Plasma (Asia Pacific)
In this Application News, a simple, fast and highly sensitive method for quantitative determination of atorvastatin in human plasma is described. The LC/MS/MS used is LCMS-8060 with a heated ESI, coupled with UHPLC Nexera X2. The high sensitivity and robust interface design of the system allow the use of protein-precipitation only in plasma pre-treatment and achieve a LLOQ of 40 pg/mL.
View here (738516 KB)

LCMS-8060 Application - Integration of steroids analysis in serum using LC-MS/MS with full-automated sample preparation (Japan)
Currently sample preparation for the detection of steroids in serum by liquid chromatography-mass spectrometry (LC-MS/MS) involves complex offline extraction methods such as solid phase extraction or liquid/liquid extraction, all of which require additional sample concentration and reconstitution in an appropriate solvent. These sample preparation methods are time-consuming, often taking 1 hour or more per sample, and are more vulnerable to variability due to errors in manual preparation. Our approach to offering a high sensitivity steroid detection method and timely, automated analysis of multiple samples is to use the automated sample preparation system coupled to the detection capabilities of a high-sensitivity triple stage quadrupole mass spectrometer.
View here (682898 KB)

LCMS-8060 Application - A high Sensitivity LC/MS/MS Method with QuEChERS Sample Pre-treatment for Analysis of Aflatoxins in Milk Powder Samples (Singapore)
A high sensitivity LC/MS/MS method with QuEChERS for sample pre-treatment was established using Shimadzu LCMS-8060 system. The QuEChERS sample preparation method was proven effective and easy to operate. The method performance including sensitivity, linearity, repeatability, matrix effect and recovery were carried out and the results con rm that the method is feasible and reliable for determination of a atoxins in milk powder samples.
View here (364871 KB)

LCMS-8060 Application - High-sensitivity, high-throughput quantitation of catecholamine metabolites in urine by LC/MS/MS for clinical research (Japan)
Catecholamines and other neurotransmitters in circulation are readily metabolized to give vanillylmandelic acid (VMA), homovanillic acid (HVA) or 5-hydroxyindolacetic acid (5-HIAA), which are excreted to urine at much higher abundance than their precursor molecules. Given this and also the non-invasive nature of sample collection, urinary neurotransmitter metabolites are growing research target in clinical context. Our aim in this study is to accelerate clinical research by providing a fast and robust LC/MS/MS method for determining urinary neurotransmitter metablites VMA, HVA, and 5-HIAA
View here (399230 KB)

LCMS-8040 Application - Development of LC/MS/MS Method for Screening and Quantitation of 47 Synthetic Dyes under Restricted Substance List in Textiles (Asia, Singapore)
A fast and highly sensitive LC/MS/MS method has been developed on LCMS-8040 for screening and quantitation of 47 restricted or banned synthetic dyes, including 23 azodyes, 21 disperse dyes and 3 basic dyes. The total run time of the method is less than 20 mins. The LOQs of the method for these dyes are at 0.1~4.1 ng/mL, which are fully complied with the current regulatory requirements.
View here (255530 KB)

LCMS-8050/8060 Application - Shimadzu Pesticide MRM Library Support for LCMSMS (UK)
To help expand capabilities in LC/MS/MS pesticide monitoring programs we have created the Shimadzu Pesticide MRM Library. The Library has been created with 766 certified reference standards and has been verified for use with Shimadzu LCMS-8050 and 8060 systems. The library contains information that can be used to accelerate method development in LC/MS/MS pesticide analysis.
View here (684018 KB)

Rapid SCreening and Quantitation of Pesticide Residues in Cannabis by Modified QuEChERS and LC-MS-MS
Medical and recreational use of marijuana (Cannabis spp.) is expanding in the United States at a rapid pace, and domestic production has increased more than ten-fold in the last 25 years. This extremely high value crop is vulnerable to mold and insects so growers frequently apply pesticides and antifungals to protect their plants. These chemical residues may pose a danger to consumers, so highly sensitive and selective methods for their detection in the complex cannabis matrix are required. We developed a rapid and effective LC-MS-MS method with modi#31;ed QuEChERS sample preparation for detection of nearly 200 chemical residues in dried cannabis #30;ower and used the method to test a wide selection of products offered for commercial sale.
View here (2083456 KB)

LCMS-8060 Application - Evaluation of the pharmacokinetics of a novel anti-diabetic agent using conventional LC/MS/MS
The ATP-sensitive potassium (KATP) channel in pancreatic b-cells is a validated anti-diabetic drug target to stimulate insulin secretion. We recently identified a novel thiosemicarbazide compound by in silico screening in combination with phenotypic screening followed by chemical modifications. The compound possesses a high stimulatory effect on insulin secretion both in vitro and in vivo through inhibition of the KATP channels. The compound significantly suppressed a rise in blood glucose levels after oral glucose load in wild-type mice in a dose-dependent manner. In this report, we analyzed pharmacokinetic profiles including dynamics of plasma concentration of compound after its oral administration using a conventional LC/MS/MS.
View here (373125 KB)

LCMS-8060 Application - Shimadzu's Guide to US EPA Method 537: Determination of Selected Perfluorinated Compounds in Drinking Water Using the Triple Quadrupole LCMS-8060 (SSI)
EPA Method 537 is a solid phase extraction (SPE), liquid chromatography/tandem mass spectrometry (LC-MS/MS) method for selected Perfluorinated Compounds (PFCs) in drinking water. This paper presents an evaluation of the instrumental portion of the method using the Shimadzu LCMS-8060 triple quadrupole mass spectrometer. The LCMS-8060 is Shimadzu’s most sensitive LC-MS/MS. Calibration ranges and estimated detection limits were well below method requirements. In addition, the chromatography was shortened from the 25 minutes in EPA 537 to less than 10 minutes without loss of resolution.
View here (835436 KB)

Integration of steroids analysis in serum using LC-MS/MS with full-automated sample preparation
Currently sample preparation for the detection of steroids in serum by liquid chromatography-mass spectrometry (LC-MS/MS) involves complex of#31;ine extraction methods such as solid phase extraction or liquid/liquid extraction, all of which require additional sample concentration and reconstitution in an appropriate solvent. These sample preparation methods are time-consuming, often taking 1 hour or more per sample, and are more vulnerable to variability due to errors in manual preparation. Our approach to offering a high sensitivity steroid detection method and timely, automated analysis of multiple samples is to use the automated sample preparation system coupled to the detection capabilities of a high-sensitivity triple stage quadrupole mass spectrometer.
View here (667135 KB)

LCMS-8050 Application - A High Sensitivity Method for Quantitative Determination of Ten Phenols in Surface Water on LC/MS/MS with APCI Interface (Japan)
A MRM-based LC-APCI-MS/MS method with fast gradient elution of 8 minutes was established and evaluated for detection and quantitation of ten phenols in surface waters. The limits of detection (LOD) of the method achieved are better than 0.1 µg/L for each individual compound except phenol and 2,4-MP, which LODs are at 1.0 µg/L. The high sensitivity of the method for the eight substituted phenols offers the possibility to determine them quantitatively and directly without the need of pre-concentration. For phenol and 2,4-MP, it requires at least ten times of pre-concentration before analysis.
View here (422355 KB)

LCMS-8050 Application - Quantification performance of non-invasive LC-MS/MS analysis and evaluation of undifferentiated state of human iPS cells
Pluripotent stem cells (PSCs) have an unlimited self-renewal capacity, and can differentiate into any cell type in the body. They consequently hold great promise as a source of cells for applications in regenerative medicine and drug discovery. For these applications, development of technology for the mass production of high quality pluripotent stem cells is essential. To contribute to development and commercialization of regenerative medicines and drug discovery, we have aimed to establish a method for the evaluation of undifferentiated state of PSCs without cell disruption. We have developed a simultaneous analysis method for 95 compounds in basal medium and secreted metabolites using liquid chromatography-tandem mass spectrometry (LC-MS/MS).
View here (528739 KB)

LCMS-8060 Application - Multi-residue analysis of 18 regulated mycotoxins by LC-MS/MS in food samples
In this work, a single LC-MS/MS method has been developed for the determination of 18 mycotoxins in food safety. Limits of quantification were at or below the maximum levels set in the EC/1886/2006 document. The scope of the method included aflatoxins (B1, B2, G1, G2), fumonisins (B1, B2, B3), ochratoxin A (OTA) and trichothecenes (3-acetyldeoxynivalenol (3AcDON), 15-acetyldeoxynivalenol (15AcDON), deoxynivalenol (DON), diasteoxyscripanol (DAS), fusarenon-X (FUS X), HT-2, neosolaninol (NEO), nivalenol (NIV), T2, zeareleonone (ZON)) with an analysis cycle time of 12.5minutes.
View here (782629 KB)

LCMS-8050 Application - Development of Sensitive and Selective Methods for Identification of Marine Toxins by LC-MS/MS
Over many decades, marine toxins have been monitored by the mouse bioassay (MBA) for the food safety purpose in many countries. In place of MBA, liquid chromatography (LC) with mass spectrometry (MS) is expected to use for the analysis of the marine toxins, deemed superior to the MBA in the point of sensitivity and accuracy. Our purpose is establishment of the analytical conditions using Liquid Chromatography Tandem Mass Spectrometry for three groups of marine toxins of which each structure and property is different.
View here (467541 KB)

Unique On-line SFE-SFC-MS/MS for Pesticides Reduces Sample Preparation & Analysis Time while Increasing Sensitivity & Polarity Range
The goal of this poster is to address four areas of improvement for pesticides analysis using on-line Supercritical Fluid Extraction – Supercritical Fluid Chromatography – Mass Spectrometry/Mass Spectrometry (SFE-SFC-MS/MS). Those areas are reduced sample preparation time, faster separation of analytes, increased sensitivity, and analysis of a wider range of analyte polarities. Sample preparation can be reduced from a 35 minute QuEChERS method to a 5 minute method with the patented on-line SFE-SFC interface. Polar compounds typically analyzed by LC-MS/MS can be analyzed faster by SFC-MS/ MS. Sensitivities can be improved over LC-MS/MS methods with the new multi-patented splitless backpressure regulator (BPR). In addition, SFE-SFC-MS/MS enables analysis of a wider range of compounds from non-polar to polar than currently available by GC-MS/ MS or LC-MS/MS. The whole process can be fully automated by adding a 48 sample rack changer on the front end.
View here (1223565 KB)

HPLC/UHPLC Method Transfer Application - Effective Analysis Management Achieved by Method Transfer between HPLC and UHPLC
High performance liquid chromatography (HPLC) is widely used for the qualitative and quantitative analysis. In recent years, ultra-high performance liquid chromatography (UHPLC) has been developed signi cantly. Facilities that have both UHPLC and HPLC systems often apply newly established UHPLC method to ordinary HPLC as well as applying existing HPLC method to UHPLC. During such inter-system method application, the method must be modi ed properly to meet the requirements from another system. This modi cation is called “method transfer”. Method transfer requires to modify existing parameters such as ow rate and/or time program. Here, we describe the relationship between column dimensions including particle size of packing material and analytical conditions, then method transfer from HPLC to UHPLC for high speed analysis and that from UHPLC to HPLC for generalization of analytical conditions as well as that from Shimadzu’s system to other vendor’s. We also describe the Shimadzu integrated LC system “Nexera-i MT” that supports method transfer and ACTO (Analytical Conditions Transfer and Optimization) Function equipped in the latest LabSolutions LC software.
View here (235750 KB)

LCMS-8060 Application - Application of SFC-MS/MS for the quantification of highly polar pesticides in a range of food samples
The analysis of highly polar pesticides by LC-MS/MS is typically achieved by several specific methods with limited chemical space. The EU Reference Laboratories for Residues of Pesticides Single Residue Methods (EURL-SRM) have published QuPPe (Quick Polar Pesticides) methods for the simultaneous analysis of a number of highly polar pesticides which cannot be easily analysed using routine QuEChERS based extraction methods and multi-residue methods (M. Anastassiades et al; QuPPe of EURL-SRM (Version 9.1; 2016). To meet the needs of analysing highly polar pesticides by LC-MS/MS several chromatographic conditions have been used including hydrophilic interaction liquid chromatography (HILIC), zwitterionic-type mixed-mode, normal-phase columns operated in HILIC-mode (bare silica and silica-based chemically bonded columns (cyano and amino)), reversed-phase C18 and carbon based phases. In this work SFC-MS/MS was applied to the analysis of a panel of highly polar pesticides extracted from several food matrices by QuPPe.
View here (697773 KB)

Anion Analysis of Ophthalmic Irrigation Solutions with the Shimadzu Prominence IC System
Ophthalmic solutions suitable for eye irrigation, eye strain relief, contact lens storage and tear replacement abound in the marketplace. While some of these serve as convenient agents for administering medicines in minute quantity, many are formulated to act as cleaning agents and may contain only dissociated ions like chloride or sulfate and organic preservatives such as benzalkonium chloride. The physiologic pH of blood and tears is approximately 7.4, but a pH range of 6.5 to 8.5 will prevent damage to the cornea. This is accomplished using buffers. To prevent eye tissue damage and maximize comfort, solutions are made to be iso-osmotic (equal osmotic pressure) with tears. The common term for this is isotonic. A 0.9% NaCl solution in pure water is said to be isotonic with tears. In this application note we will aid in the quality control of such ophthalmic solutions for their content of common anions.
View here (574925 KB)

LCMS-IT-TOF Application - High Speed, High Resolution Analysis (Part 25) High Resolution Analysis of BSA Digest (Japan)
The MALDI-TOF mass spectrometer can detect ions that are formed due to fragmentation within the ion source (ISD, In-Source Decay). When ISD occurs in analysis of proteins, primarily it is the c-type ion (Fig. 1) of the N-terminus that is detected. Up to now, 2,5-dihydroxybenzoic acid (DHB) has been used widely as a matrix for inducing ISD, but recently, 1,5-diaminonaphtalene (DAN) has been reported to be a more effective matrix in this regard (see References). Amino acid sequence information is easily acquired by detection of ISD ions using DAN, and highly homologous proteins can be investigated using homology searches.
View here (2992624 KB)

Nexera Application - Ultrafast, Ultra High-Sensitivity Analysis of Aflatoxins
"Nucleotides, building blocks of DNA and RNA, are compounds where phosphate(s) bond to a nucleoside that is composed of a nucleobase and sugar. In general, adenine (A), cytosine (C), guanine (G), thymine (T), and uracil (U) are examples of nucleobases, and ribose and deoxyribose are examples of sugar. There are many other types of nucleotides depending on the number of bonding phosphates (1 to 3).      For high-separation analysis of these components, a long column with a particulate packing material can be used. However, both the UHPLC unit and column need to have a high pressure-resistance. This document introduces an example of ultrahigh separation analysis performed on nucleotides using Nexera, which is resistant to 130 MPa, and a Shim-pack XR-ODS III column (particle size 2.2 µm), resistant to 100 MPa."
View here (199876 KB)

Nexera Application - High Speed, High Resolution Analysis (Part 41) Performance Evaluation of Carryover Using Reserpine in Human Plasma by the Nexera UHPLC System
To ensure quality control and safety in manufacturing facilities within the pharmaceutical industry, it is important that cleaning validation be conducted following the cleaning of production-related equipment to ensure the quantity of residual substances collected from the surfaces of the equipment are within permissible limits. For this cleaning validation using a TOC analyzer, the following 3 types of methods are available. (1) Rinse sampling – TOC measurement method (2) Swab sampling – aqueous extraction – TOC measurement method (3) Swab sampling – direct combustion carbon measurement method Introduced here are the features of each of these methods, using the TOC-LCPH total organic carbon analyzer (Shimadzu Corporation, Kyoto, Japan), in the measurement of residual pharmaceutical products and their constituent substances.
View here (1271207 KB)

Detection of Non-Separated Impurities by i-PDeA
When optimizing the separation conditions to be used for quantitation and fractionation of the principal components of a sample, the goal is to produce a reliable separation between the main components and impur i t ies , including minor co-component s . A photodiode array detector is useful for confirming the presence of unexpected impurities and co-components because each has a different spectral pattern. By using i-PDeA (Intelligent Peak Deconvolution Analysis), the UV spectrum obtained by the photodiode array detector is derivatized to remove the principal components so that only the impurities remain visible in the data trace. It is a function that permits more reliable detection of impurities than that offered by the conventional peak purity method, and allows efficient optimization of the separation conditions. Here, we introduce the detection and resolution of unseparated peaks using the high-sensitivity SPD-M30A photodiode array detector in conjunction with the i-PDeA function of LabSolutions.
View here (1133296 KB)

High Speed, High Resolution Analysis (Part 46) Analysis of Pre-Column Derivatized Biogenic Amines by the Nexera SIL-30AC Autosampler
Biogenic amines are produced naturally by the enzymatic decarboxylation of amino acids in beverages and food. Biogenic amines such as these are also used as an indicator of food spoilage. Histamine, a substance that can cause allergy-like food poisoning, must not exceed 50 ppm in food in general according to FDA standards, 100 ppm in marine products in the EU, and 400 ppm in fish sauce according to the Codex International Food Standards. In addition, biogenic amines such as cadaverine and tyramine appear to intensify the allergy-like food toxicity of histamine. In Application News articles L432 and L437, we introduced examples of the pretreatment functions of the SIL-30AC autosampler in the analysis of fluorescence-derivatized amino acids us ing o-phthalaldehyde (OPA). Here, we introduce an example of the analysis of fluorescent amines that were derivatized with OPA.
View here (1149693 KB)

HPLC Application - Analysis of Cold Medicine Using Newly Developed Shim-Pack MAqC ODS I column
In Application News No. L459, we introduced the simultaneous analysis of water-soluble vitamins using the Shim-pack MAqC-ODS I column. Use of the Shim-pack MAqC-ODS I column makes it possible to achieve retention of highly polar basic compounds without the use of ion-pair reagents in the mobile phase, thereby permitting the application of gradient elution. As a result, improved sensitivity and time savings can be achieved in the simultaneous analysis of highly polar basic compounds and other substances. Similarly, to water-soluble vitamins, pharmaceutical substances also contain many basic compounds having high solubility in water. Here, using the Shim-pack MAqC-ODS I column, we introduce an example of analysis focusing on substances that are typically included as active ingredients in over-the-counter cold medicines.
View here (970172 KB)

Nexera-e Application - Comprehensive Two-Dimensional Analysis of Polyphenols in Red Wine Using Nexera-e Coupled with SPD-M30A
Phenolic compounds are created as secondary metabolites in plants. In many cases, their structures contain multiple aromatic rings and a hydroxyl group. These polyphenols are known to display antioxidant effects, and are said to be effective in preventing arteriosclerosis and cerebral infarction. Red wine is known to contain large amounts of polyphenols, including flavonoids and phenolic acids, and in recent years has attracted considerable attention due to the health benefits associated with these substances. Regarding the analysis of polyphenols in red wine, separation and quantitation of these polyphenols by simultaneous analysis using HPLC is difficult due to the presence of many coexisting substances. The Nexera-e comprehensive two-dimensional liquid chromatograph can be very effective for such an analysis.
View here (947190 KB)

LCMS-2020 Application - Analysis of Polysorbate 80 in IgG Aqueous Solutions by Online SPE Using Shim-Pack MAYI Column Part 1 (Japan)
The Japanese Ministry of Health, Labour and Welfare (JMHLW) specified in July 1980 that the mouse bioassay (MBA) be used as the official method for diarrhetic shellfish toxin, and that the permissible exposure limit be 0.05 MU per gram of edible shellfish. Shellfish in which the toxin exceeds this limit are prohibited from being sold at market according to the Japanese Food Sanitation Law. Due to significant technological advances since 1980, the sensitivity and accuracy obtained using the MBA method are significantly inferior compared to the high-precision, high-sensitivity possible using liquid chromatography mass spectrometry analytical instrumentation, which is currently used for this application. A complete transition to instrumental analysis for lipophilic marine biotoxins is scheduled to be implemented by January 2015 throughout the EU.
View here (1232137 KB)

LCMS-IT-TOF Application - Comprehensive 2D Separation of Triglycerides in Vegetable Oil with ELSD/LCMS-IT-TOF Detection
When conducting comprehensive two-dimensional liquid chromatography, different separation modes are generally selected for the first and second-dimension separations, and depending on the differences in separation selectivity between these dimensions, improved separation is typically seen for components that are difficult to separate in a single, one-dimensional analysis. Here, suing borage oil as a sample that contains many triglycerides, micro-scale separation was conducted in the first separation using a silver column (normal phase conditions), and reversed phase separation was conducted in the second dimension by using a two-liquid gradient with non-aqueous organic solvents. Detection was conducted using a combination of an evaporative light scattering detector (ELSD) and an ion trap time-of-flight mass spectrometer (LCMS-IT-TOF).
View here (1411372 KB)

Nexera-I LC2040C 3rd Party Application – Improving the Consistency and Accuracy of Tetracyclines Regulatory Laboratory Testing of Contaminated Beef, Chicken, and Cow’s Milk with Simple Automation (Horizon)
Tetracyclines are one of the most commonly used antibiotic agents in the United States. A majority of the usage is for agricultural purposes, where it is estimated 80% of tetracyclines administered is for disease prevention in healthy animals. They are also used in farming to keep animals raised in close proximity healthy and gaining weight. In 2012, the FDA indicated, tetracycline accounted for 41 percent of the 31 million pounds of antibiotics sold for farm animals in the United States. While the use of tetracyclines is very beneficial for the production of agriculture products, there are concern about long term adverse health effects for humans. Evidence has shown repeated exposure to low levels of tetracyclines through food sources has lead to antibiotic resistant pathogens. Antibiotic resistance to one drug may transfer to another, especially those within the same drug class. Also, repeated exposure to antibiotics could cause the development of allergies to these compounds, especially in children.
View here (1471552 KB)

LCMS-8030 Application - Improvement in Suppression of Carryover of Auto-Sampler for High Sensitivity MS Detector (Japan)
As the sensitivity of the mass spectrometer has been greatly improved, the carryover of the sample remaining in the auto-sampler has become the most significant factor determining the quantitative performance of the whole LC-MSMS system. Meanwhile, as the demands arise for faster speed and higher resolution of the analysis, the higher-pressure HPLC has become available from many HPLC venders. However, users sometimes experience carryover problem in higher-pressure system that they have not experienced with conventional HPLC system pressure. We have studied how the carryover performance is affected by the system pressure, and in this paper we report how we can improve carryover in a higher-pressure application.
View here (727217 KB)

Nexera Application - Fast and High Sensitivity Analysis of Six Preservatives in Beverages by UHPLC with Photodiode Array Detection
Food preservatives are additives to inhibit, retard or prevent mould, acidification or other deterioration of foodstuffs caused by microbial contamination. The most commonly used preservatives in beverages are benzoic acid, sorbic acid and four parahydroxybenzoic acid esters (parabens). However, excess amounts of these additives can be harmful to consumer health. In this regard, the minimum permissible concentrations of preservatives are regulated in most countries to ensure safety for consumer. Therefore, quantitative analysis of these preservatives in food is not only required for food quality assurance but also important for consumer interest and protection. High performance liquid chromatography (HPLC) has been used for analysis of the preservatives in beverage. In this Application News, a new rapid and high sensitivity UHPLC method for simultaneous determination of the six preservatives in beverages is described. A gradient elution was optimized for separation and quantitation of the six preservatives with a photodiode array detector. A capillary flow cell with extra long optical path of 85 mm was employed to achieve high sensitivity for a very small injection amount of sample (1mL) which was not cleaned up except filtration.
View here (347652 KB)

HPLC Application - Determination of Polyether Antibiotics in Animal Feeds (Part 1) Analysis by Post-Column VIS Photometric Derivatization Method
Five kinds of polyether antibiotics, including salinomycin sodium, are specified as feed additives based on the 750th notification of Japan's Ministry of Agriculture, Forestry and Fisheries, for addition to the feeds of domestic cattle and poultry to promote growth through the effectiveness of the nutritional content of these feeds. Analysis of these compounds in feed is conducted using microbiological quantitation methods and HPLC methods, as listed in the “Feed Analysis Standard”. HPLC allows more rapid analysis compared with microbiological quantitation methods, with postcolumn derivatization and VIS detection specified for four of the compounds and fluorometric detection specified for one of the compounds. Here we introduce an example of analysis of salinomycin sodium (SL), monensin sodium (MN), narasin (NR) and senduramicin sodium (SD) using the post-column derivatization VIS method, as specified.
View here (208637 KB)

HPLC Method Transfer Application - Improving Method Transfer by Adjustment of Gradient Delay
In facilities that have number of high performance liquid chromatography (HPLC) systems, an existing method that gives proper result by one HPLC system is often applied to other HPLC systems (method transfer). However, due to the difference in system volume, pump characteristics, and liquid delivery mechanisms among systems, method transfer can yield different results even though the same method is used. In this report, we rst explain the gradient delay due to the system volume difference and the effect of the delay on separation. We then show an example of method transfer with adjustment of gradient delay using alkylphenones and UV absorbents as samples. We also describe the integrated liquid chromatograph (LC) system "i-Series" that supports to optimize method transfer and the newly designed function of "Analytical Conditions Transfer and Optimization (ACTO) " equipped in the latest version of LabSolutions software.
View here (166756 KB)

i-Series Application - Analysis of 1, 2, 3-Benzotriazole in Electrical Insulating Oil with Prominence-i
Electrical insulating oils are used widely in oil-immersed transformers and oil-filled capacitors. When abnormal heating or insulation degradation occurs inside oil-filled equipment, gas produced by decomposition of the insulating oil and products of insulator deterioration will mix with the insulating oil and change its chemical properties. Quantitation of 1, 2, 3-benzotriazole is used as a method for testing the performance of insulating oil. 1, 2, 3-benzotriazole is often added to electrical insulating oil to suppress streaming electrification during cooling, and prevent sulfidation corrosion. It is also known to improve thermal stability and electrical properties. The method used to quantify 1, 2, 3-benzotriazole in electrical insulating oils is described in JIS C 2101 "Testing methods of electrical insulating oils." An example analysis of 1, 2, 3-benzotriazole in electrical insulating oil is described here using the new Prominence-i integrated high performance liquid chromatograph.
View here (85527 KB)

Nexera UC Application - Analysis of Choline and Acetylcholine in Rat Cerebrospinal Fluid Samples Using the Nexera UC-MS/MS System (Japan)
Choline, which is a structural element of cell membranes, and acetylcholine, which is known as a neurotransmitter, are both familiar compounds in the field of bioanalysis. Since acetylcholine is biosynthesized in the body from choline, it is possible to estimate the quality of internal activity by monitoring both of these compounds. This article focuses on the SFC analysis of these compounds in a rat cerebrospinal fluid sample by direct injection of the cerebrospinal fluid to the Nexera UC SFC system. Also introduced is automatic extraction and analysis of a cerebrospinal fluid sample impregnated into filter paper, in consideration of convenience and durability for storage and transport, using the Nexera UC online SFE-SFC-MS/MS system.
View here (312116 KB)

LCMS-8040 Application - Highly Sensitive and Robust LC/MS/MS Method for Quantitative Analysis of Artificial Sweetners in Beverages (Asia Pacific)
Melamine was found to be used as a protein-rich adulterant rst in pet-food in 2007, and then in infant formula in 2008 in China. The outbreak of the melamine scandal that killed many dogs and cats as well as led to death of six infants and illness of many had caused panic in publics and great concerns in food safety worldwide. Melamine was added into raw milk because of its high nitrogen content (66%) and the limitation of the Kjeldahl method for determination of protein level indirectly by measuring the nitrogen content. In fact, in addition to melamine and its analogues (cyanuric acid etc), a number of other nitrogen-rich compounds was reported also to be potentially used as protein-rich adulterants, including amidinourea, biuret, cyromazine, dicyandiamide, triuret and urea. Recently, low levels of dicyandiamide (DCD) residues were found in milk products from New Zealand. Instead of addition directly as an adulterant, the trace DCD found in milk products was explained to be relating to the grass “contaminated by DCD”. Dicyandiamide has been used to promote the growth of pastures for cows grazing. We report here an LC/MS/MS method for sensitive detection and quanti cation of both dicyandiamide (DCD) and melamine in infant milk powder samples.
View here (600167 KB)

LCMS-8050/8060 Application - Enhancing Ion Sampling Efficiency, Ion Transmission and Detection on a Triple Quadrupole Platform (Japan)
For the past decades marine toxins in shell fish have been monitored by the mouse bioassay (MBA) in many countries including Japan. Recently several alternative testing methods have been developed and a few of them have been validated. The most widely accepted method for many kinds of the marine toxins is liquid chromatography (LC) combined with mass spectrometry (MS), deemed to be the powerful tool than the MBA in sensitivity and accuracy. Diarrhetic shell fish poisoning (DSP) toxins, okadaic acid (OA) and dinophysistoxins (DTXs), are very important target for marine bio-toxin monitoring in Japan. The MBA for DSP toxin monitoring was replaced with a LC/MS/MS method on the new regulation issued in March 2015 in Japan (Notification No. 1 issued by the Dept. of Food Safety, Pharmaceutical and Food Safety Bureau, Japanese Ministry of Health, Labour and Welfare on March 6, 2015). In this presentation, we demonstrate the developed LC/MS/MS methods for the screening of OA, dinophysistoxin1 (DTX1), pectenotoxin1, 2, 6 (PTX) and yessotoxin (YTX) as well as for the routinely quantification of OA and DTX1.
View here (904644 KB)

LCMS-8040 Application - High Sensitive Detection and Quantification of Thirty-Two Synthetic PDE-5 Inhibitors and Analogues Adulterated in Health Supplements Using LC/MS/MS (Asia Pacific)
In recent years, synthetic phosphodiesterase type 5 enzyme (PDE-5) inhibitors like sildena l (active component of VIAGRA) were found as adulterant in some health supplements described as plant or herbal products. Only seven synthetic PDE-5 inhibitors, namely, sildena l, tadala l, vardena l, avana l, udena l, mirodena l and lodena l carbonate are approved officially to be used for the treatment of erectile dysfunction (ED) in men. The adulteration is illegal and may be also dangerous for consumers, because not only the above PDE-5 inhibitors, many newly appeared analogues that are synthesized with minor modification of the parent structures are also found used as adulterants. Analytical techniques like HPLC and LC/MS/MS have been applied for screening and quantitation of PDE-5 inhibitors and their analogues. We describe here a high sensitivity LC/MS/MS method for detection and quantification of thirtytwo synthetic PDE-5 inhibitors and analogues spiked in health products.
View here (233942 KB)

LCMS-8040 Application - Characterization and Isolation of Quinones from Tectona Grandis Linn. leaves using Innovative Hyphenation of TLC-MS interface with LC/MS/MS System (India)
Tectona grandis Linn. (T. grandis Linn.) (Family -Verbenaceae) is commonly called as ‘teak’ and locally known as ‘sagwan’ and one of the most famous timber plants in the world. This plant is well known for its dimensional stability, extreme durability and hardness which also resist decay even when unprotected by paints and preservatives. A variety of interesting but limited compounds have been isolated and identified from T. grandis Linn. still more study needs to be performed especially for its color components which mainly includes quinones. HPTLC technique is used for the separation of phytochemicals, followed by its identification using LC and LC/MS/MS system. Traditional introduction of sample from TLC plate to MS is cumbersome and time consuming. The new TLC-MS interface by CAMAG, Switzerland has made it possible to have online transfer of a fraction from TLC plate to MS. The feature of ‘optimisation of method’ present in LCMS-8040, provides qualitative confirmation of compounds w.r.t. standards.
View here (774412 KB)

MALDI-Resonance Application - Phosphorylation Analysis by MALDI-TOF MS (5) -Identification of a Phosphoprotein (Japan)
Here we introduce an example of the analysis of 6-gingerol and 6-shogal, constituents of ginger, using the Prominence UFLC ultra fast LC system with the SPD-M20A photodiode array detector.
View here (1427444 KB)

Development of a LC-QIT-TOF mass spectrometer capable of high mass accuracy and stability.
The combination of QIT-TOF with an ESI source has been developed using novel ion introduction optics. Instrument performance characteristics have now been extensively investigated in regards to mass accuracy and stability.
View here (362 KB)

Fractionation of Anthocyanins by Preparative LC-MS System
Anthocyanins are the flavonoid color pigments present in all tissues of higher plants, including the petals and leaves.Besides their use as food dyes, anthocyanins have recently attracted attention due to their antioxidant properties.
View here (468 KB)

MALDI-Confidence Application - Protein Sequencing Using In-Source Decay (Japan)
Here we present an example of high speed, high resolution analysis of phenolic acids using the Shimadzu Prominence UFLCXR ultra high-speed LC system with the SPD-M20A photodiode array detector.
View here (1389725 KB)

GC Application - High Temperature Simulated Distillation using Shimadzu GC-2010
Here we introduce an example of high-speed analysis of α-acids and β-acids in hops using the Prominence UFLCXR ultra fast, high resolution LC system with a high-speed, high-resolution column.
View here (675212 KB)

LC/MS Analysis of Perfluorochemicals (PFCs) Using Impurity Delay Method
Using the LCMS-2020 with its excellent sensitivity and repeatability and its newly developed QoQ ion optical system, together with the impurity delay method, allows 0.1 μg/L trace-level quantitative analysis of PFOA and PFOS with excellent repeatability.
View here (670985 KB)

Impurity Analysis of Highly-Polar Compounds Without Using Ion-Pair Reagents
Ion-pair reagents which contain fluorine are often used for LC/MS; however, as ion-pair reagents tend to accumulate in the column, interface, switching to another separation mode may take a considerable amount of time to allow complete flushing of the residual ion-pair reagents. Here we introduce analytical conditions that do not include the use of an ion-pair reagent.
View here (1436074 KB)

ICP Application - Fertilizer Analysis by ICPE-9000
Here, we introduce the results of analysis of MG modification of heat shock protein Hsp27 in response to various stresses (acidification, chemical substances, etc.) using the Prominence nano-AccuSpot-AXIMA Performance LC-MALDI system. It is notable that several new modification were found during this experiment.
View here (1010894 KB)

Analysis of Methylglyoxal-Modified Heat Shock Protein 27 Using C-MALDI System
In this application we introduce the results of analysis of MG modification of the heat shock protein Hsp27 in response to various stresses (acidification, chemical substances, etc.) using the Prominence nano-AccuSpot-AXIMA® Performance LC-MALDI system. It is notable that several new modifications were found during this experiment.
View here (1295257 KB)

TOC Application - TOC-V - Measurement of Oil Residues on Copper Wire Surface by TOC Solid Sample Measurement System
Here, we introduce an example analysis of a mixture of synthetic quinolone antibacterials using the Nexera ultra high performance LC system with the RF-20Axs high-sensitivity fluorescence detector.
View here (1157529 KB)

MALDI-Performance Application - Differentiating βAsp Residue by PSD in a Curved Field Reflectron (Japan)
Here, we introduce the results of the carryover evaluation of the Nexera SIL-30AC autosampler using the Nexera UHPLC (Ultra High Performance Liquid Chromatography) System and LC/MS/MS.
View here (1359382 KB)

Analysis of Polymer Additives Using the LCMS-8030 Triple Quadrupole LC/MS/MS
Antioxidants, ultraviolet absorbers, flame retardants and other polymer additives are indispensable for improving the characteristics and functionality of polymers. Understanding the types and quantities of these additives to be used is extremely important to effectively control the manufacturing process of the polymers. Below is an example of quantitative analysis of 14 types of polymer additives using MRM (Multiple Reaction Monitoring) and the LCMS-8030 triple quadrupole mass spectrometer.
View here (1431769 KB)

Analysis of Serotonin using LC-MS-MS
Serotonin is an important neurotransmitter responsible for feelings of mood and cognitive functions, sleep, and appetite. Many pharma-ceuticals target pathways related to serotonin. The structure of serotonin is shown in Figure 1. Analytical methods to measure serotonin are needed to study the effects of this important neurotransmitter.
View here (719650 KB)

ICP Application - Analysis of Sewage and Sewage Sludge by ICPE-9000
Here, we introduce the quantitative analysis of 3-MCPD fatty acid esters in palm oil using LC/MS/MS. Synthetic 3-MCPD-dipalmitoyl ester and 3-MCPD-dioleoyl ester were used as standard samples.
View here (809903 KB)

Qualitative Analysis of Tochu Tea Using a Triple Quadrupole LC/MS/MS [LCMS-8030]
The LCMS-8030 triple quadrupole mass spectrometer is used in qualitative analysis to conduct precursor ion scans to search for precursor ions that produce common product ions, and to conduct neutral loss scans to detect ions that dissociate to common neutral fragments. Here, we describe the precursor ion scan in the search for active ingredients in Tochu tea using the LCMS-8030.
View here (847460 KB)

Analysis of 3-MCPD Fatty Acid Diesters in Palm Oil Using a Triple Quadrupole LC/MS/MS [LCMS-8030]
This application note illustrates that it is possible to use a triple quadrupole mass spectrometer for detection of 3-MCPD fatty acid esters using a simple pretreatment procedure that is limited to sample dilution.
View here (997585 KB)

Analysis of Perchlorate in Water by Non-Suppressed Ion Chromatography-Mass Spectrometry
Perchlorate is a chemical substance that occurs both naturally and as a manufactured compound, and is used in a wide range of applications. It is a common accelerant in rocket engines and an explosive in the pyrotechnics industry. From the standpoint of health, however, it is now suspected to be associated with hypothyroidism. A non-suppressed single LC/MS system is a low-cost, easy-to-operate system for monitoring perchlorate in water such as factory wastewater.
View here (997378 KB)

LCMS-8040 Application - Multi-class pesticides analysis in challenging vegetable matrices using fast 5 msec MRM with 15 msec polarity switching (Japan)
In this study, we developed an LC-based approach to determine metabolite profiles including polar metabolites and to identify specific endogenous components, aiming at high throughput and comprehensive methods using TOFMS acquisition.
View here (186760 KB)

High Throughput LC-MS-MS Analysis of Carbendazim in Orange Juice
Highly sensitive analytical methods are necessary to prevent contaminated produce from entering the food supply. This poster showcases the development of an ultrafast UHPLC-MS-MS method for analysis of carbendazim in orange juice using a new high-speed UHPLC autosampler in tandem with a newly developed high-sensitivity triple quadrupole mass spectrometer.
View here (418659 KB)

Analysis of Hemoglobin Variants using an Automated Sample Preparation Workstation Coupled to LC-MS
There are over 2000 known hemoglobin variants, and it is important to be able to structurally identify and quantitate them quickly and precisely. This poster presents a quick, reproducible method of identifying differences between normal and abnormal hemoglobin utilizing an automated sample preparation system, which reduces sample complexity, coupled to mass spectrometry.
View here (1374645 KB)

LCMS-8030/8040 Application - Quantitation of Pesticides in Fruits and Vegetables using a Fast Scanning and MRM-LCMS Method (SSI)
A rapid LC-MS-MS method for detection of oil dispersants in water was developed.
View here (2482190 KB)

AA Application - A459: Measurement of Metal Ion in Plating Solution by Flame Atomic Absorption
An analytical LC-MS-MS method to measure serotonin is demonstrated to provide a way to study the effects of this important neurotransmitter.
View here (1126388 KB)

LCMS-8040 Application - Queued and Ready to Run? Testing the Stability of Vitamin Extracts While in Queue Using Triple Quadrupole LC/MS/MS Analysis (SSI)
An HPLC-MS/MS method was developed for the profiling and quantitation of corn stover hydrolyzate samples for known phenolic fermentation inhibitors.
View here (245064 KB)

Application of Metabolomics Techniques using LCMS and GCMS Profiling Analysis of Green Tea Leaves
This Application Note presents the profiling of green tea leaves as an example of one application of the metabolome analysis technique using LC/MS and GC/MS. A search of the substances believed to play roles in product quality was conducted, and a quality prediction model was constructed based on the results.
View here (677590 KB)

In Wine There is Truth - The Characterisation and Quantitative Analysis of Wine Using Spectroscopic Methods (Germany)
Here we report the simultaneous measurement of 97 metabolites by triple quadrupole LC/MS/MS using penta uorophenylpropyl column. In this experiment, MRM transitions of these metabolites were optimized and this method was applied to biological samples. Furthermore, to evaluate the accuracy of developed method for quantification, simultaneous analysis by PFPP column was compared to measurement of ion-paring chromatography.
View here (313379 KB)

LCMS-8040 Application - Highly Sensitive Quantitative Estimation of Genotoxic Impurities from API and Drug Formulation using LC/MS/MS (India)
In this study, we developed a methodology which enabled the automated procedure of pre-column chiral derivatization of D- and L- amino acids.
View here (483346 KB)

LCMS-8050 Application - Rapid determination of beta-agonist residues in animal tissues using UHPLC-tandem mass spectrometry including mass spectral library searching (UK)
The objectives of the current studies were to develop a selective and sensitive LC-MS/MS method to determine of telbivudine in human plasma.
View here (374435 KB)

LCMS-8050 Application - Quantitative Analysis of Anabolic Steriods in Control Samples from Food-Producing Animals Using a Column-Switching LC-HESI-MS/MS Assay (UK)
Here we introduce the analysis results of single and mixture samples with both the particle size distribution and the light intensity distribution.
View here (1111641 KB)

LCMS-8050 Application - Tetrahydrocannabinol (THC) analysis in oral fluids using the LCMS-8050 (SSI)
This Application News introduces the use of the LCMS-8050 triple quadrupole mass spectrometer for analysis of these HAAs in accordance with the official LC/MS methodology requirements.
View here (522591 KB)

LCMS-8050 Application - Analysis of Haloacetic Acids in Drinking Water Using Triple Quadrupole (Japan)
The aim of this study was to develop a fast, sensitive and simple methodology for a range of challenging highly polar pesticides that require single-residue methods, by as few multi-residue LC-MS/MS runs as possible and without the need for derivatisation.
View here (860934 KB)

LCMS-8050 Application - Haloacetic acids in drinking water by LCMS (Japan)
This Application News introduces the use of the LCMS-8050 triple quadrupole mass spectrometer for analysis of these HAAs in accordance with the official LC/MS methodology requirements.
View here (856786 KB)

ICP Application - ICP Analysis of Drinking Water
Here, we introduce an example of phenol analysis by UHPLC/MS/MS. Unlike the use of GC/MS for this analysis, LC/MS/MS does not require derivatization, and therefor simplifies the analysis process.
View here (1043883 KB)

GCMS-QP2010 Ultra Application - Analysis of Phthalate Esters Using the PY-Screener (2) (Japan)
This paper describes an LC-MS/MS method for high-sensitivity simultaneous analysis of the four compounds, nivalenol, deoxynivalenol and deoxynivalenol metabolites, 3-acetyl-deoxynivalenol and 15-acetyl-deoxynivalenol.
View here (217191 KB)

Analysis of Impurities in Pharmaceutical Ingredients Using Trap-Free Two-Dimensional HPLC and Triple Quadrupole LC/MS/MS (LCMS-8040)
In this report, we introduce an example of analysis in which trap-free two-dimensional HPLC was used to detect impurities using non-volatile mobile phase conditions, which were then converted without complication to volatile mobile phase conditions online to complete the analysis using the LCMS-8040 triple quadrupole mass spectrometer.
View here (1526525 KB)

Simultaneous Analysis of 36 Veterinary Drugs using Triple Quadrupole LC/MS/MS
This report illustrates the simultaneous analysis of 36 veterinary drugs measured in 15 minutes using the Shimadzu LCMS-8050 Ultra Fast Triple Quadrupole Mass Spectrometer, featuring ultrafast polarity switching. The polarity switching speed of the LCMS-8050 is just 5 milliseconds.
View here (214546 KB)

Checking for meat authenticity using targeted LC-MS/MS analysis
In this work previously published proteotypic peptides were selected to detect horse, pork, beef and chicken using Skyline software (MacCoss Lab Software - University of Washington). These were used to interrogate a Uniprot database FASTA download for myosin (43263 proteins) and collagen (44531 proteins) to determine no other species cross reactivity to pig myosin and collagen.
View here (902544 KB)

Enhanced Sensitivity for Assay of Sulfonamide Drugs and Trimethoprim in Honey by LCMS Triple Quadrupole Mass Spectrometry with QuEChERS Extraction
Twenty one sulfonamides along with trimethoprim were analyzed by LC-MS/MS using a Nexera HPLC system coupled to an LCMS-8060 triple quadrupole mass spectrometer. Diverse clean up sorbents for extraction and purification were tested using a QueChERS method.
View here (1341568 KB)

High-Speed Analysis of Sunitinib and Axitinib in Plasma Using Triple Quadrupole LC/MS/MS (LCMS-8050)
This article introduces an example measurement of the molecularly targeted drugs sunitinib and axitinib using the LCMS-8050 high-sensitivity triple quadrupole mass spectrometer. Although a simple method of sample pre-treatment was used that involves only deproteinization, the quantitative results obtained were excellent in terms of accuracy and precision.
View here (923546 KB)

High-Speed Analysis of Mycophenolic Acid in Plasma Using Triple Quadrupole LC/MS/MS (LCMS-8050)
This article introduces an example of high-speed analysis of mycophenolic acid in plasma using the LCMS-8050 high-sensitivity triple quadrupole mass spectrometer. Although a simple method of sample pretreatment was used that involves only deproteinization, the quantitative results obtained were excellent in terms of accuracy and precision.
View here (974564 KB)

LCMS-8050/8060 Application - Shimadzu Pesticide MRM Library Support for LCMSMS
To help expand capabilities in LC/MS/MS pesticide monitoring programs we have created the Shimadzu Pesticide MRM Library. The Library has been created with 766 certified reference standards and has been verified for use with Shimadzu LCMS-8050 and 8060 systems.
View here (665253 KB)

High-sensitivity, high-throughput quantitation of catecholamines and metanephrine in plasma by automated WCX-SPE coupled to LC/MS/MS for clinical research
Catecholamine levels in plasma, namely norepinephrine (NE), epinephrine (E) and dopamine (DA), give indication of disease states and are routinely measured for clinical research. Recently, plasma catecholamine metabolites such as metanephrine (MN) and normetanephrine (NMN) are increasingly studied as an alternative of or to complement catecholamine levels. Therefore high-sensitivity and high-throughput analytical system that covers all of these compounds is warranted.
View here (452658 KB)

Separation of Tricyclic Antidepressants Using Pathfinder Columns at Acidic Conditions
View here (217 KB)

Determination of Cimetidine in Pharmaceutical Tablets by High Performance Liquid Chromatograpy
View here (121 KB)

A Simple HPLC Method for the Detection of Preservatives in Inks
View here (118 KB)

Separation of Nucleotide Acid Bases with Reversed Phase Chromatography under Aqueous Mobile Phase Conditions
View here (122 KB)

Peptide Separation Using a Polymer Encapsulated Reversed Phase Column
View here (145 KB)

Steric Selectivity of Pathfinder Columns According to Tanaka and Enhelhardt
View here (139 KB)

Simultaneous Determination of Thirteen UV Filters in Sunscreen Products
View here (131 KB)

Quantification of Acetylsalicylic Acid and ist Related Substance Salicylic Acid
View here (130 KB)

A Rapid Method for the Determination of Amiodarone and ist Metabolite Desethylamiodarone
View here (127 KB)

Computer-assisted Optimizatiuon in the Development of a HPLC method for the analysis for Amines
View here (186 KB)

Column Classification and Selection of Pathfinder stationary phases with embedded Polar Groups
View here (229 KB)

Realization of HPLC Methods by using Computer Assisted Method Development
View here (223 KB)

Efficient separation and accurate spotting of NBS Labeled Peptides Using the Micro HPLC AccuSpot System
View here (108 KB)

Analysis of Dietary Supplements
Analytical Instrumentation & Software for the Evaluation, Identification and QA/QC of Dietary Supplements
View here (811787 KB)

Analysis of Golf Course Pesticides Using Triple Quadrupole LC/MS/MS (LCMS-8030)
Many kinds of pesticides are used to maintain golf course turf, and because golf courses are often located in mountain corridors and near water sources, pollution of nearby fresh water sources and tap water from golf course waste water is of concern. With this increased concern over the environment, in 1990 Japan's Ministry of the Environment issued the "Provisional Guidance Indicators for the Prevention of Water Pollution from Pesticides Used in Golf Courses" (hereafter, Guidance Indicators), in which indicator values were specified for 21 pesticides. Then, a notification issued on September 29, 2010 increased the list to 72 pesticides and made it a requirement to conduct simultaneous analysis of the chemicals using higher sensitivity instruments. Of those 72 pesticides, we conducted simultaneous analysis of 21 of the remaining 44 substances specified to be evaluated by LC/MS using the LCMS-8030, and in addition, we conducted monitor testing of golf course wastewater. The results are presented here.
View here (1308603 KB)

GCMS-QP2010 Ultra Application - Paint Thinner Analysis Utilizing Headspace GCMS (Japan)
When using the two dimensional LC system introduced here, retention time repeatability in the first dimension is extremely important because impurity peak fractionation is conducted within specific time-controlled intervals. In other words, this technique cannot be applied unless retention times are consistent. However, it is reasonable to assume that the repeatability of retention times has already been determined since retention time repeatability is fundamental to the development of a specific test method. If the separation technique for the first dimension separation is already established, measurement can be conducted without re-evaluation of the technique introduced here, eliminating the need for LC/MS measurement using complex volatility conditions that would have been required otherwise. The ability to confirm impurities through comparison with blank data should greatly contribute to the efficiency of CMC impurity identification.
View here (139423 KB)

LCMS-8030/8040 Application - Analysis of phthalate esters in environmental water samples by online-SPE-LC coupled with high-speed triple quadrupole mass spectrometer (Japan)
The application of atmospheric pressure ionization sources in mass spectrometry necessitates the presence of a differential pumping system in order to maintain high vacuum in the analyzer. Commercial triple quadrupole mass spectrometers typically have from 3 to 4 differential pumping stages and an RF ion guide is generally utilized as a ion focusing device in the higher pressure region of the ion path. The ions generated under atmospheric pressure need to be efficiently focused to minimize the loss of ions prior to introduction into quadrupole analyzer by use of an RF lens system. Using a QqQ with 4 differential pumping stages, we have investigated the application of a fringing field in the RF ion guides installed in the second and third differential pumping stages with a resultant improvement in sensitivity by a factor of five.
View here (264087 KB)

LCMS-8030/8040 Application - High throghput analysis of anion surfactant using ultra-high speec LC-MS/MS and 1 mm inside diameter column (Japan)
In recent years the need for forensic, toxicological and clinical analyses have increased, and as a consequence of sample complexity, analysis has become increasingly challenging due to a growing trend in the use of illicit drugs and non-medicinal prescription drugs. Screening applications requires rapid and unambiguous results that can be achieved using a generic analysis method designed for a large number of target compounds. To meet this need, a universal high speed MRM triggered product ion scanning method with fast polarity switching was applied to simultaneously screen, quantitate and confirm by reference to an MS/MS data base containing the majority of drugs of abuse available in Japan.
View here (242777 KB)

LCMS-8030 Application - High Throughput Quantitative Analysis of Multi-mycotoxin in Beer-based Drinks using UHPLC-MS/MS (Japan)
Aflatoxins (AFs) are the most harmful mycotoxins produced by the fungi Aspergillus flavus and Aspergillus parasiticus and can contaminate foods such as cereals and nuts. To reduce the risk of the ingestion from foods, analyses of the AFs are carried out in many countries. It is necessary to quantitate the total aflatoxin (B1, B2, G1, G2) in foods by the regulation in JAPAN. The conventional LC/MS method proposed by the Ministry of Health, Labour and Welfare of Japan has a total analysis time of 30 minutes. In this study, we examined two alternative high-throughput LC-MS/MS methods. The first optimized for sensitivity & quantification; the second, a rapid screening method, using UHPLC for the purpose of increasing work flow.
View here (395297 KB)

LCMS-8030/8040 Application - SAMHSA Drugs of Abuse Urinary conrmation for 11 drugs by LC-MS-MS (SSI)
A comparison was made in 2000 for analysis of total dissolved nitrogen (TDN) in seawater samples; a report from which is “in press” in Marine Chemistry. In that comparison, 30 independent analyses of five prepared marine samples with varying contributions from dissolved inorganic nitrogen (DIN) and organic nitrogen (DON) were completed. That comparison included 7 TDN analyses by UV irradiation, 13 by persulfate oxidation, and 9 by high temperature combustion (HTC) methods. The overall variability from the 30 analyses ranged from 8-28% (coefficient of variation for one standard deviation). At that level of variability, no method or instrument could be deemed inadequate for complete analysis of TDN. The HTC methods, as a family, showed tighter agreement and the most promise for ease of future analyses and were therefore investigated further.
View here (822415 KB)

LCMS-IT-TOF Application - Fragmentation Outcome Modelling: Prototype Software for Prediction of CID Fragment Ions for Small Molecule Structures (SEG)
Surfactant chemistry makes affect to a number of household products including detergents, shampoos and toothpaste. Anionic surfactants have been widely distributed throughout the water environment via household effluent. LAS (linear alkylbenzene sulfonate) is the commonest in various kinds of anionic surfactants. As the presence of LAS in environmental water can seriously affect aquatic organism, it is necessary to monitor the concentration of LAS in environmental water. In case that it may be present at trace level, sample preparation have generally been conducted such as the solid phase extract (SPE) and concentration. In this study, automation of the sample preparation using online SPE LC system coupled with LC-MS/MS was developed for the determination of LAS concentration in environmental water.
View here (1080218 KB)

LCMS-8040 Application - Applying Micro Flow LC and High Speed Data Acquisition MS/MS to the Analysis of Pesticides Residues in Complex Spice Matrix (UK)
Over 50 cytotoxic chemotherapies are used in hospitals. The main anti-cancer drugs used in cancer chemotherapy can be classified into several categories: cytotoxic, the most represented, but also hormones, immune response modifiers and antibodies. Most cytotoxic agents used in cancer chemotherapy interact with DNA or its precursors. Very few studies are evaluating the future of these drugs in wastewater. Potential risks associated with these discharges are poorly understood and require study work and research to better understand the hazards, exposure characterization and assessment risks to human health and the environment. The purpose of the study is to establish an analytical methodology to screen most of the anti-cancer drugs currently used in hospital waste waters.
View here (756034 KB)

LCMS-8040 Application - Simultaneous Analysis of Hydrophilic Metabolites Using Triple Quadrupole LC/MS/MS (Japan)
The toxicological assessment of Genotoxic Impurities (GTI) and the determination of acceptable limits for such impurities in Active Pharmaceutical Ingredients (API) is a dif cult issue. As per European Medicines Agency (EMEA) guidance, a Threshold of Toxicological Concern (TTC) value of 1.5 µg/day intake of a genotoxic impurity is considered to be acceptable for most pharmaceuticals. Dronedarone is a drug mainly used for indications of cardiac arrhythmias. GTI of this drug has been quantitated here. Method has been optimized for simultaneous analysis of DRN-IA {2-n-butyl-3-[4-(3-di-n-butylamino-propoxy)benzoyl]-5-nitro benzofuran}, DRN-IB {5-amino-3-[4-(3-di-n-butylamino-propoxy)benzoyl}-2-n-but yl benzofuran} and BHBNB {2-n-butyl-3-(4-hydroxy benzoyl)-5-nitro benzofuran}.
View here (328083 KB)

LCMS-8050 Application - Rapid Analysis of Immuno-suppressants using Triple Quadrupole LC-MS/MS (Japan)
In a method development of quantitative proteomics, thousands of MRM are needed to be monitored to exhaustively pursue an optimum condition. Skyline1 can simplify the workflow for both method set up and data processing. On the other hand, in typical triple quadrupole mass spectrometers, it is mandatory for users to divide the experiment into multiple methods to monitor over a thousand MRMs with adequate sensitivity. In other words, multiple injections are required which wastes time and precious samples. Shimadzu UFMS features an ultra fast MRM analysis (UF-MRM®) capability which enables the reduction of number of injections. Figure 1 illustrates an example of method development with trypic digest of BSA by using a single injection. A total of 1710 MRM transitions were monitored in 8 minutes. By combining intuitive features of Skyline and UF-MRM® of Shimadzu UFMS LCMS-8050, the throughput in quantitative proteomics is greatly improved.
View here (622216 KB)

LCMS-2020 Application - Analysis of Sulfamic Acid in Fertilizers Using LC/MS (Japan)
Industrial fermentation for the production of biofuels or biopharmaceutics requires routine monitoring of medium conditions such as pH, dissolved gas, carbon source (glucose) and nitrogen source (glutamine) for optimization and control of the fermentation process. However, culture media also consist of various other biologically important compounds such as vitamins, nucleic acids, and other primary metabolites, which would lead to more detailed understanding of the bioprocess if monitored altogether. To meet the demand for comprehensive analysis of medium component, we optimized the analytical conditions and developed this “Method Package for Cell Culture Profiling” that can monitor relative abundance of 95 compounds listed herein. Using this Method Package, we demonstrated the change in abundance of culture medium components associated with hybridoma growth over a period of 5 days.
View here (946410 KB)

LCMS-8040 Application - LC-MS/MS Analysis of the New Antioxidant Identified from a Soft-Body Extract of Crassostrea Gigas (Japan)
Analysis of pesticide residues in food is typically tedious and time-consuming due to the necessary extraction and clean up procedures. Furthermore, to deal with the ever-growing number of pesticides, the food safety laboratories need to ideally screen as many compounds as possible in a single run which may reach maximum residual limits (MRL); typically 10 ppb in food matrices. In this study, we illustrate the results utilizing an UF MRM capability (just 5 msec. MRM measurement includes dwell and pause time) with 5 msec. polarity switching (UF switching) for the analysis of 146 pesticides in crude food extracts by using easy and simple sample preparation technique.
View here (888932 KB)

LCMS-8050 Application 3rd Party - Determination of Minodronate in Rat Plasma By LC-MSMS (China)
Norepinephrine (NE), serotonin (5-HT) and dopamine (DA) play important roles as neurotransmitters and are classical biomarkers for diseases such as hypertension and neuroblastoma. To improve the detection sensitivity of these monoamines is a primary challenge especially for microdialysis study. One of many approaches for improving the sensitivity of monoamine detection by LCMS is a derivatization of monoamines to attach a hydrophobic moiety so that they retain better on reverse-phase columns. While this approach is effective from a chromatographic point of view, the extent of this effect on the overall sensitivity of detection depends on ionization efficiency and ion transmission in mass spectrometry, which vary amongst instrument type due to different architecture. We compared herein the sensitivity and background noise level associated with neurotransmitter quantitation by Shimadzu and AB Sciex instruments.
View here (11998964 KB)

LCMS-8050 Applicaiton - EU Workplace Drug Testing by Dilute and Shoot LC-MS/MS with Enhanced MRM Data Quality (UK)
In this study we present a single dilute and shoot methodology using a high sensitivity triple quadruple mass spectrometer in order to meet the required European Work Place Drug testing cut-off concentrations (and other international regulatory guidelines, e.g. SAMSHA). A comprehensive suite of drugs were studied including amphetamines, benzodiazepines, opiates, cannabis, barbiturates, cocaine, methadone, and some of their metabolites. This list included amobarbital, pentobarbital, phenobarbital, secobabital and butalbital which are typically difficult to incorporate into multi-residue methods due to low sensitivity and the required chromatographic separation of structural isomers amo/pentobarbital. To enhance data quality the method was optimized to acquire 6 MRM transitions for each compound, rather than the conventional 2 MRMs
View here (92659 KB)

LCMS-8050 Application - High Throughput Simultaneous Analysis of 39 Amino Acids in Various Foods without Derivatization using LC-MS/MS (Japan)
As amino acids in foods are essential components of nutrition and taste, it is expected to develop an easy and efficient analytical method. Amino acids are highly polar compounds, so it needs their derivartization or addition of ion-pair reagent in mobile phase in order to separate them by reversed phase mode. In the case of hydrophilic interaction chromatography, it may be difficult to separate isomers or to analyze comprehensively. In our previous study we developed a simultaneous analysis method of 20 amino acids by LC-MS/MS with mix-mode column (ion exchange and normal phase), without derivartization. In this study, we tried to increase the number of targeted amino acids (39 amino acids), and detected them in various foods with high sensitivity.
View here (1119829 KB)

Analysis of Sulfamic Acid in Fertilizers Using LC/MS (LCMS-2020)
Sulfamic acid, due to its plant growth inhibiting effects, is subject to maximum limits in fertilizers as specified in the official standard1) for ordinary fertilizers according to the Japanese Fertilizers Regulation Act. According to the Testing Methods for Fertilizers2) supervised by Japan's Food and Agricultural Materials Inspection Center (FAMIC), the ion chromatography (IC) method is specified as the test method for sulfamic acid in ammonium sulfate. It has been reported, however, that when applying this IC method with byproduct compound fertilizer (fertilizer produced by concentrating and drying liquid byproducts obtained from fermentation plants involved in amino acid production, etc.) samples that contain large amounts of organic matter, it is difficult to separate the sulfamic acid peaks from contaminant peaks generated from sample matrix.3) In this application, we investigated the analytical conditions for LC/MS that would permit acquisition of mass information and provide high selectivity in order to eliminate the effects of contaminating components. The LCMS-2020 single quadrupole mass spectrometer was used for the analysis.
View here (925456 KB)

High Speed Analysis of Haloacetic Acids in Tap Water Using Triple Quadrupole LC-MS/MS
Haloacetic acids (HAAs), by-products of water disinfection, are formed from naturally-occurring organic and inorganic materials in water which react with the disinfectants chlorine and chloramine. Certain haloacetic acids have been shown to cause adverse reproductive or developmental effects in laboratory animals. Three HAAs regulated by numerous government bodies such as the US EPA include chloroacetic acid (CAA), dichloroacetic acid (DCAA) and trichloroacetic acid (TCAA). A Liquid Chromatography Mass Spectrometry (LC-MS/MS) method for measuring HAAs capable of direct injection of water samples has been developed to replace previously used methods requiring tert-butyl-methyl ether liquid extraction and diazomethane derivitization prior to GC analysis, thus reducing the effort required for sample preparation. Reduced sample preparation times combined with rapid UHPLC chromatography increase the productivity of water control laboratories. This data sheet illustrates results from a high speed method acquired using a LCMS-8050 triple quadrupole mass spectrometer coupled with a Nexera X2 UHPLC.
View here (409545 KB)

LCMS-8050 Application - Analysis of Residual Chloramphenicol in Shrimp by LC/MS/MS with QuEChERS Sample Pre-treatmen (Asia Pacific)
Chloramphenicol (CAP) is a broad spectrum antibiotic that is widely used in the growth of animals and marine culture. However, CAP can cause aplastic anaemia and is a possible carcinogen in humans. Its use in livestock farming including fish and shrimps has been banned in European Union and many other countries. However, illegal use of CAP is still present due to its low cost and ready availability. As there is not a safe maximum residue level (MRL) determined in food for CAP, a highly selective and sensitive analytical method to detect CAP residues in complex matrices such as food samples is required. Here, we present a LC/MS/MS method for accurate and reliable quantitation of CAP in shrimp samples on LCMS-8050 with a heated ESI interface. The shrimp samples were pre-treated with a modified QuEChERs procedure. The method performance was evaluated with spiked samples and exhibits good accuracy, reproducibility, linearity and specificity over the concentration range from 0.005-20 ng/mL.
View here (275641 KB)

LCMS-8060 Application - Selective and sensitive quantification of glucagon and glucagon-related peptide hormones in human plasma using conventional LC/MS/MS (Japan)
Impaired secretion of endogenous bioactive peptides such as peptide hormones and cytokines is associated with the development and pathophysiology of various diseases. Glucagon is a peptide hormone known to increase blood glucose levels. Glucagon-like peptide 1 (GLP-1), a peptide hormone generated from the same precursor as glucagon, regulates glucose metabolism by enhancing insulin secretion from pancreatic β-cells. Because of similarities between amino acid sequences of glucagon and glucagon-related peptides derived from proglucagon, the quantification of glucagon in blood by conventional immunoassay methods have been hampered by cross-reactivity of anti-glucagon antibodies with glucagon-related peptides. In the present study, to selectively quantify these peptide hormones in human plasma, we developed a sensitive method using a LC/MS/MS.
View here (548325 KB)

LCMS-8050 Application - A Fast LC/MS/MS Method for High Sensitivity Determination of Twenty-Six Perfluorocompounds in Textiles (Asia)
A sensitive and reliable LC/MS/MS method has been developed for screening and quantitation of 26 PFCs including PFOA and PFOS on Shimadzu LCMS-8050 UFMS system. The method adopted M-PFOA (13C-PFOA) as internal standard to enhance the reliability for screening analysis of unknown sample. The LOQs of the MRM method achieve extremely low level, e.g., 17.7 and 16.1 ng/mL for PFOA and PFOS in textile matrix, respectively. The method performance which includes sensitivity, linearity, repeatability, matrix effect and recovery were evaluated. The results indicate that the method is feasible and reliable for determination of 26 targeted PFCs, especially PFOA and PFOS in different textile samples.
View here (240870 KB)

LCMS-8060 Application - Expanding Capabilities in Multi-Residue Pesticide Analysis Using the LCMS-8060 (UK)
A fast, selective and highly sensitive method has been developed for the quantitation of 646 pesticides using a single method with 1919 transitions (corresponding to up to 3 MRM transitions per compound) and a LC gradient time of only 10.5 minutes. As the LCMS-8060 has a rapid polarity switching time of 5 msec, the single multi-residue LC/MS/MS method supported the analysis of 34 pesticides in negative ion mode and 612 compounds in positive ion mode. The enhanced performance and higher sensitivity of the LCMS08060 has created new opportunities in sample dilution to reduce ion signal suppresion and matrix effects. For most compounds a dilution factor of 1:20 or 1:50 was sufficient to provide recoveries in the range of 70-120%
View here (1444400 KB)

LCMS-8040 Application - Trace level quantitative determination of pthalates from high risk dosage pharmaceutical formulations using LC/MS/MS
Phthalates are plasticizers which fi#30;nd their use in variety of applications like packaging material in pharmaceutical preparations, plastic toys, personal-care products etc. Since they are used as additives, they can leach out from the polymeric matrix. Studies have demonstrated that phthalates exposure can cause endocrine disruption, cancer, autism etc. These hazards make it mandatory to quantify phthalates especially in high risk dosage pharmaceutical formulations which act by directly affecting the site of action in the body. Hence a highly sensitive LC/MS/MS method has been developed for trace level quantitative determination of phthalates from high risk dosage pharmaceutical formulations using LCMS-8040, a triple quadrupole mass spectrometer from Shimadzu Corporation, Japan.
View here (518720 KB)

LCMS-8060 Application - Evaluation of the pharmacokinetics of a novel anti-diabetic agent using conventional LC/MS/MS (Japan)
The ATP-sensitive potassium (KATP) channel in pancreatic b-cells is a validated anti-diabetic drug target to stimulate insulin secretion. We recently identified a novel thiosemicarbazide compound by in silico screening in combination with phenotypic screening followed by chemical modifications. The compound possesses a high stimulatory effect on insulin secretion both in vitro and in vivo through inhibition of the KATP channels. The compound significantly suppressed a rise in blood glucose levels after oral glucose load in wild-type mice in a dose-dependent manner. In this report, we analyzed pharmacokinetic profiles including dynamics of plasma concentration of compound after its oral administration using a conventional LC/MS/MS.
View here (400212 KB)

LCMS-8050 Application - Rapid Screening and Quantitation of Pesticide Residues in Cannabis by Modified QuEChERS and LC-MS-MS (SSI)
Medical and recreational use of marijuana (Cannabis spp.) is expanding in the United States at a rapid pace, and domestic production has increased more than ten-fold in the last 25 years. This extremely high value crop is vulnerable to mold and insects so growers frequently apply pesticides and antifungals to protect their plants. These chemical residues may pose a danger to consumers, so highly sensitive and selective methods for their detection in the complex cannabis matrix are required. We developed a rapid and effective LC-MS-MS method with modified QuEChERS sample preparation for detection of nearly 200 chemical residues in dried cannabis ower and used the method to test a wide selection of products offered for commercial sale.
View here (2132982 KB)

LCMS-8060 Application - Protein biomaker quantitation from human blood and plasma using novel collection technology by LCMS/MS (UK, France)
The growth and broad adoption of dried blood spots (DBS) has been driven by the simplicity of the technique for collection, storage and transport of the samples. Its simplicity has resulted in its widespread use in predominantly small molecule applications such as therapeutic drug monitoring and toxicology although DBS has been used in HIV for monitoring antiretroviral (ARV) therapy and in mass spectrometry-based proteomics the focus has been on the analysis of haemoglobin. The limitations of DBS relate not only to sample stability, variable haematocrit levels and matrix effects in the LC-MS/MS analysis but also with the presence of erythrocytes (in the case of ARV therapy proviral DNA leads to an overestimation of viral load). Dried plasma spots (DPS) sampling provides an alternative approach to DBS possibly negating the effect of the haematocrit and reducing matrix effects in LC-MS/MS analysis. This paper compares the distribution of proteins in samples collected by DBS and DPS.
View here (468266 KB)

Analysis of Residual Chloramphenicol in Shrimp by LC/MS/MS with QuEChERS Sample Pre-treatment
We present a LC/MS/MS method for accurate and reliable quantitation of CAP in shrimp samples on LCMS-8050 with a heated ESI interface. The shrimp samples were pre-treated with a modified QuEChERs procedure. The method performance was evaluated with spiked samples and exhibits good accuracy, reproducibility, linearity and specificity over the concentration range from 0.005-20 ng/mL. The quantitation limit of the method with 5μL injection volume are determined to be 0.01 ng/mL, which is equivalent to 0.2 μg/kg of CAP in shrimp samples after incorporating a dilution factor of 20 from the sample pre-treatment procedure. This value satisfies the Minimum Required Performance Limit (MRPL) set at 0.3 μg/kg by the European Union.
View here (270546 KB)

LCMS-8050 Application - Comprehensive Analysis of Primary and Secondary Metabolites in Citrus Fruits Using an Automated Method Changeover UHPLC System and LC/MS/MS System (Japan)
Metabolome analysis, which is the comprehensive analysis of all metabolites present in a living organsim, is now being apploed in a variety of areas and not just to analyze the metabolites of living organisms. Metabolome analysis is becoming an important tool in the food sector in areas such as food processing and plant breeding. In food analysis, it is very important to carry out comprehensive analysis of primary and secondary metabolites that contribute to the color, smell, taste, and functional properties of food. To date, there has been only a few examples of performing these anlyses simultaneously. In this article, we describe a method of performing comprehensive analysis of primary and secondary metabolites in food (major organic acids, amino acids, sugars, carotenoids, and flavonoids) using LC/MS/MS, and also present an example application of this analytical method using citrus fruits as an actual sample.
View here (2293479 KB)

LCMS-8050 Application - Simultaneous Analysis of 16 Sweeteners Using Triple Quadrupole LC/MS/MS (Japan)
Artificial sweeteners such as aspartame, sucralose, and acesulfame potassium fall under the category of designated additives according to Japan's Food Sanitation Act, and prescribed standards are in place for their use in some foods and quantities. Cyclamate and other artificial sweeteners used in some regions outside Japan are included among undesignated additives in Japan, and inspection is required in specific imported foods. Consequently, quantitation for large numbers of sweeteners, including not only permitted in Japan but also undesignated, are needed. Application News C121 described the simultaneous analysis of nine artificial sweeteners including both designated and undesignated additives using an LCMS-8040 triple quadrupole LC/MS/MS system. In this article, we introduce an example of simultaneous analysis of 16 sweeteners using an LCMS-8050.
View here (82059 KB)

LCMS/GCMS Application - Classification of Beer Types Using Metabolic Profiling (Japan)
In food science, global metabolite analysis, or ‘metabolomics’, is increasingly applied to a number of value-added food production areas including food-safety assessment, quality control, food authenticity, origin and processing. GC-MS/MS and LC-MS/MS are widely used for measuring the total amount of metabolites in a sample. Selection of the appropriate instrument to be used is based on the target compounds and the objective. In this study, a mass spectrometry–based metabolomics approach was applied to differentiate and classify five types of beer (two lager beers, an ale type beer, a beer-taste alcoholic beverage and a beer-taste non-alcoholic beverage). GC-MS/MS and LC-MS/MS techniques were used to target amino acids, organic acids, sugar and nucleic acid-related compounds which are known to be the compounds associated with sweetness, bitterness and perceived flavor in food and beverages. Statistical analysis of the detected compounds by PCA and HCA clearly differentiated five types of beer.
View here (774870 KB)

LCMS-8060 Application - High Sensitivity Analysis of Pesticides in Dried Hops Cones and Hops Pellets by Liquid Chromatography- Triple Quadrupole Mass Spectrometery (SSI)
Hops (Humulus lupulus) are an essential ingredient in brewing beer but agricultural production of this plant is threatened by insects and other dangers. Pesticides and other chemicals may be used to protect hops and increase yield, but certain chemical residues may be harmful to consumers. Chemical residues may also have unintended negative effects on non-target insects such as honeybees. Sensitive and selective detection of chemical residues in hops is necessary to ensure protection of consumers and the environment. Methods using LC-MS provide efficient and effective detection of chemical residues in a complex sample matrix such as hops. We have developed an LC-MS method for detection of over 150 analytes in hops and carried out a market survey of over 50 different hops pellets samples.
View here (2250008 KB)

LCMS-8060 Application - Multi-Residue Analysis of 18 Regulated Mycotoxins by LC/MS/MS (UK)
Mycotoxins are one of the most important contaminants in food and feed due to their widespread distribution in the environment and toxic effects on humans and animals. Structurally, mycotoxins are a very diverse group with a wide range of physicochemical properties and low molecular weights. They are produced by fungi (mould) frequently found on agricultural produce, and are often not visible to the naked eye. Some of the most commonly contaminated food stuffs include wheat, oats, rye, corn, barley, rice, nuts and milk. Due to the risks posed by mycotoxins in food they are regulated globally, including, the EU, US, China, Singapore and Brazil. In the EU, reporting limits are harmonised in Regulation (EC) No 1886/2006 (amended by (EC) No 1126/2007) and sampling and analysis in Regulation (EC) No 401/2006. LC/MS/MS is the technique most commonly employed for mycotoxin quantitation in order to achieve the necessary low reporting limits in complex food and feed matrices.
View here (76391 KB)

LCMS-8060 Application - High Sensitivity Analysis of Pesticides in Dried Hops Cones and Hops Pellets
Hops (Humulus lupulus) are an essential ingredient in brewing beer but agricultural production of this plant is threatened by insects and other dangers. Pesticides and other chemicals may be used to protect hops and increase yield, but certain chemical residues may be harmful to consumers. Chemical residues may also have unintended negative effects on non-target insects such as honeybees. Sensitive and selective detection of chemical residues in hops is necessary to ensure protection of consumers and the environment. Methods using LC-MS provide efficient and effective detection of chemical residues in a complex sample matrix such as hops. We have developed an LC-MS method for detection of over 150 analytes in hops and carried out a market survey of over 50 different hops pellets samples.
View here (2181546 KB)

Improved sensitivity for characterization of sulfonamides and trimethoprim in honey using QuEChERS extracts with LC-MS/MS.
Improved sensitivity for characterization of sulfonamides and trimethoprim in honey using QuEChERS extracts with LC-MS/MS.A natural food as honey is subject of diverse restrictions for contaminants presence as the case of antibiotics including sulfonamides. It is a worldwide practice by Beekeepers to use antibiotics as therapeutic agents to treat bee bacterial brood diseases, however the use of sulfonamides (SA) and trimethoprim (TMP) in beekeeping practice is prohibited in EU. There are no a worldwide MRL’s for sulfonamides in honey in the EU, but a minimum required performance level (MRPL) was set for analytical methods at a level of 10 μg/kg of sulfonamides, encouraging the development of reliable laboratory methods for detection in diverse foods included honey. SAs and TMP posing threats to public health causing allergic reactions and increasing microorganism’s drug resistance. Considering MRLs and MRPL of SAs and TMP in food products from animals tend to be continually reduced to preserve human health safety, HPLC-MS/MS is an effective strategy to characterize and accurately measure those antibiotics. The present method is selective, fast, and very sensitive for 20 sulfonamides and trimethoprim.
View here (199356 KB)

ICPMS Analysis - Quantitation of Arsenic Species in White Rice and Brown Rice Using LC-ICP-MS System
Rice is one of the agricultural products that incorporates a relatively significant amount of arsenic in which the ratio of inorganic to organic arsenic is known to be high. Both inorganic and organic arsenic species are known for their potential for harm, however, inorganic arsenic is known to be more toxic than organic arsenic. As such, the Codex Alimentarius Commission held in July 2014 determined 0.2 mg/kg to be the maximum concentration of inorganic arsenic in processed rice. An LC-ICP-MS system which connects an inductively coupled plasma mass spectrometer (ICP-MS) in-line with a high-performance liquid chromatography (HPLC) system allows high sensitivity and high accuracy measurement of arsenic species. This report demonstrates the quantitation of inorganic arsenic species [As(III) and As(V)] and dimethylarsinic acid in white rice and brown rice that was accomplished by connecting the Shimadzu ICPMS-2030 in-line with a HPLC system.
View here (1275241 KB)

LCMS-8050/8060 Application - Analysis of Bromate in Tap Water Using a Triple Quadrupole LC/MS/MS (Japan)
Bromate in tap water is generated by advanced water treatment processes such as ozone disinfection in the process of water purification. Potassium bromate has been classified by the IARC (1999) as a Group B2 substance which is possibly carcinogenic to humans, and was added to the water quality standards of Japan in 2004. Upon its addition, ion chromatography with postcolumn absorption spectroscopy was designated as the testing method for bromate. (Annex table 18 of "Method Determined by the Minister of Health, Labour and Welfare on the Basis of the Ordinance Provisions Relating to Water Quality Standards", Notification No. 261 issued by the Ministry of Health, Labour and Welfare of Japan (MHLW) in 2003) In December 2016, the MHLW gathered opinions for partial amendment of this method, and as given in annex table 18-2 "Liquid Chromatography-Mass Spectrometry", mass spectrometry was proposed as a new testing method (proposal) for bromate. This article introduces the results of our examination of LC/MS/MS analysis using an anion exchange column based on this new testing method (proposal).
View here (352085 KB)

LCMS-8040/8050 Application - Mice fecal metabolomics by LC-MS/MS: Comparison between young mice and old mice
The intestinal microbiome plays an important role in health and/or disease because it in uences pathological and normal homeostatic functions. Low-molecular-weight metabolites produced by intestinal microbiome are absorbed constantly from the intestinal lumen and carried to systemic circulation; they play a direct role in health and/or disease. There are limited reports concerning the function of metabolites produced by intestinal microbiome. Furthermore, these studies are targeting specific metabolites such as short chain fatty acids but not global metabolites (metabolome). For clarifying the relationship between health and/or disease and metabolome produced by intestinal bacteria, only free bacterial metabolites in the intestinal luminal content (or feces) should be analyzed. In this study, metabolites in feces of young and old mice were analyzed by LC-MS/MS.
View here (458816 KB)

A Modified INA Method for the Analysis of Milk Thistle Using
One of the widely available nutraceutical products seen in supermarkets is a powdered form of Milk Thistle or silybum marianum, derived from the plant native to Mediterranean Europe. It has been used from ancient times as a liver tonic. The milky sap produced by Milk Thistle contains flavolignans, collectively known as the silymarin group. Growing consumer interest, combined with the low cost and growing availability of herbal supplements and remedies, has driven the need for standardization of these products.
View here (32 KB)

HPLC Application - Ultra High Sensitivity Analysis Using Newly Designed Fluorescence Detector
The BioSpec-nano is a state-of-the-art UV-VIS Spectrophotometer for life sciences, ideal for quantitation of nucleic acids or fluorescently-labeled nucleic acids. Completely automated, it offers such features as ‘Drop and Click’ sample mounting-measurement, and cleaning. Manual operations such as moving the optical fiber vertically or cleaning the parts in contact with the liquid are unnecessary. This communication presents data on the accuracy and reproducibility of the BioSpec-nano for dsDNA quantitation.
View here (1017151 KB)

Applications of the Prominence RF-20AXS - Fluorescence Detector - High Sensitivity Analysis of Anionic Surfactants, tert-Butylhydroquinone, and Amitrole
The Prominence RF-20AXS fluorescence detector not only achieves high sensitivity levels never before seen (water Raman SN ratio greater than 2000), but it also features a temperature-controlled flowcell with a cooling function as standard to provide highly reliable detection unaffected by ambient temperature fluctuations. Here we introduce examples of high sensitivity analysis using the Prominence RF-20AXS.
View here (258806 KB)

Applications of the "Prominence RF-20Axs" Fluorescence Detector (Part 4) Analysis of Pesticides with a Postcolumn Derivatization System
Fluorescence detectors are widely used in the food and environmental fields due to their high sensitivity and selectivity. Among these applications, fluorescence detection is used for analysis of iminoctadine and Nmethyl carbamate pesticides in food and tap water by a post-column fluorescence derivatization method. Here we introduce examples of these analyses using the Prominence RF-20Axs fluorescence detector with the Prominence Iminoctadine Analysis System and the Prominence Carbamate Analysis System.
View here (265654 KB)

Analysis of Ginkgolic Acids in Ginkgo Biloba Extract
Ginkgo leaf extract (ginkgo biloba extract), which contains active ingredients extracted from ginkgo biloba leaves, is reported to be effective in improving cerebral and peripheral blood circulation deficiencies. It is used in Japan and the United States in the form of a dietary supplement, and in Germany, France, and other European countries as a prescription medication. However, alkylphenols which are present in the ginkgolic acids contained in ginkgo leaves are known to cause allergic reactions. For this reason, the United States Pharmacopeia (USP) has established an upper limit for ginkgolic acid content in ginkgo biloba extract. Here we introduce an example of analysis of gingkolic acids contained in ginkgo biloba leaves.
View here (435121 KB)

High Speed, High Resolution Analysis (Part 31) Analysis of Mexiletine, Pilsicainide, and Zonisamide in Serum
HPLC separation and quantitation are often used for measurement of drug concentrations in the blood. When analyzing the concentration of a drug in the blood using HPLC, the separation of contaminants and analytes requires a long analysis time. For that reason, there is demand for faster HPLC analysis to improve the productivity of drug pharmacokinetic studies and clinical testing, particularly when handling many samples. Here we introduce analyses of mexiletine, pilsicainide, and zonisamide in serum using the ultra-high speed Prominence UFLC system and high-speed Shim-pack XR-ODS separation column.
View here (220000 KB)

Applications of the Prominence RF-20Axs Fluorescence Detector (Part 5)
Voglibose is a diabetes drug which inhibits the activity of α-glucosidase. HPLC post-column derivatization is specified as the test method for voglibose in the Japanese Pharmacopeia, Fifteenth Edition (voglibose purity test, quantitation of voglibose in pharmaceutical tablets). Here we introduce an example of voglibose tablet testing as specified in the Japanese Pharmacopeia, Fifteenth Edition, using the Prominence post-column derivatization system with the Prominence RF-20Axs fluorescence detector.
View here (1161175 KB)

Applications Using "Prominence RF-20Axs" Fluorescence Detector (Part 6)
Fluorescence detectors are widely used in the environmental analysis due to their high sensitivity and high selectivity. Even trace amounts of chemical compounds often affect the ecosystem. Bisphenol A is one of such compounds for which trace-level analysis of environmental water is greately required. Here we introduce examples of high-sensitivity analysis of bisphenol A using the Prominence RF- 20Axs fluorescence detector by direct injection and by using an automated column-switching preconcentrating system.
View here (1374799 KB)

Internal Standard Addition During Pretreatment Using SIL-30AC
Data with excellent repeatability was obtained using both the internal standard "stacked injection" and the internal standard mixing and dilution pretreatment methods. The examples presented here focused on the use of the internal standard addition technique, but in the amino acid analysis example as well, the pretreatment program was utilized to demonstrate that good repeatability can be obtained without concern for even slight differences in reaction time. In particular, the more complicated the pretreatment process, the more difficult it becomes to maintain repeatability when conducting pretreatment manually. For this reason, the Nexera SIL-30AC pretreatment functions were designed to address a wide range of pretreatment processes, from automated primary screening of large numbers of samples to pretreatment requiring accurate reaction time.
View here (1508397 KB)

Analysis of Hexafluorophosphate Ionin Electrolytic Solution for Lithium-Ion Rechargeable Battery
In Application News No. L403, we introduced an example of the analysis of electrolytic solvents used in lithium-ion rechargeable batteries. Here, we will investigate the analysis of electrolytes. In order for a substance to be suitable as an electrolyte, it must dissociate in a non-aqueous solvent and be able to withstand the oxidation-reduction environment at the cathode and anode. One such typical electrolyte is lithium hexafluorophosphate. Here, we introduce an example of analysis of the hexafluorophosphate ion in the electrolytic solution used in lithium-ion rechargeable batteries by HPLC.
View here (947523 KB)

Applications Using "Prominence RF-20Axs" Fluorescence Detector (Part 6) - Analysis of Bisphenol A at High Sensitivity
Fluorescence detectors are widely used in the environmental analysis due to their high sensitivity and high selectivity. Even trace amounts of chemical compounds often affect the ecosystem. Bisphenol A is one of such compounds for which trace-level analysis of environmental water is greatly required. Here we introduce examples of high-sensitivity analysis of bisphenol A using the Prominence RF-20Axs fluorescence detector by direct injection and by using an automated column-switching pre-concentrating system.
View here (1375471 KB)

Applications of the Prominence RF-20AXS Fluorescence Detector (Part 7)High Sensitivity Analysis of Retinol Acetate and Retinol Palmitate
In everyday use, the term "Vitamin A" is synonymous with retinol. Because retinol is a substance that is easily oxidized, highly stable derivatives of retinol are used in such products as foods, medicines and cosmetics. In HPLC analysis of stable retinol derivatives such as retinol acetate and retinol palmitate, a fluorescence detector offers both selectivity as well as high-sensitivity analysis. Here we introduce examples of high-sensitivity analysis of retinol acetate and retinol palmitate, in addition to ultra-high speed analysis of retinol palmitate using the Prominence RF-20AXS fluorescence detector.
View here (1348358 KB)

HPLC Application 3rd party - Assessment of a New Generation of Evaporative Light Scattering Detectors for Liquid Chromatography: Sensitivity, Linearity, Dynamic Range, Analyte Dispersion and Response Variation with Eluent Compositions (SEDERE)
Here, we introduce an example of measurement of copper wire using the solid sample measurement system comprising the TOC-V CPH total organic carbon analyzer and the SSM-5000A solid sample combustion unit.
View here (1049287 KB)

The Perfinity Workstation: Achieving Quality through Automation
The Perfinity Workstation effectively removes the sample preparation bottleneck by automating and integrating reproducible and rapid affinity selection, sample clean-up, proteolysis and buffer exchange. All of these processes can be completed in under 10 minutes, resulting in peptide maps of exceptional reproducibility (<10% CVs). Applications of this workstation include targeted proteomics, biomarker validation and PTM analysis.The Perfinity Workstation incorporates software that is extremely easy to use, greatly reduces the learning curve and requires no method programming. The workstation allows everyday users to apply MS to proteins, integrates with current proteomics/biomarker MS workflows, dramatically reduces sample prep time, is fully automated, multiplex capable, easily customizable and requires no antibody immobilization. More information is available at Perfinity.com and PerfinityWorkstation.com.
View here (4627227 KB)

Analysis of Dye Degradation in Dye-Sensitized Solar Cell
Of the organic photovoltaic cells that have been under extensive development as next-generation solar cells, dye-sensitized solar cells are perhaps the closest to commercialization today. These types of solar cells are expected to be produced inexpensively. Commercialization will of course be contingent on sufficient photoelectric conversion efficiency, but equally important will be their endurance in withstanding degradation over time. By using HPLC, it is possible to observe changes in these dyes over time. Here we introduce some analytical examples of the degradation of one such dye, referred to as N3 dye.
View here (1272388 KB)

Shimadzu at MSACL 2012 Workshop
<p class="article"><strong> Prepare Your Lab for the Future…<br> From Automated Sample Prep to Ultrafast Mass Spectrometry</strong> </p> <p class="article">Presented at The Association for Mass Spectrometry Applications to the Clinical Lab (MSACL) 2012 conference, this workshop consists of the following presentations:</p> <p class="article"> &ndash; Achieving Truly Ultrafast UHPLC-MS-MS, Jeff Dahl, Shimadzu Scientific Instruments<br /> &ndash; The Perfinity Workstation: A Faster, More Reproducible, Fully-automated Sample Prep Platform, Kevin Meyer, Perfinity Biosciences<br /> &ndash; Integrating the Perfinity Workstation into the Biomarker Validation Pipeline for Diagnostic Assays, Christine Jelinek, Johns Hopkins School of Medicine<br /> </p>
View here (7713522 KB)

LCMS-8030/8040 Application - Nexera Application - Nexera Application - High Speed, High Resolution Analysis (Part 41) Carryover Evaluation of Glibenclamide in Human Plasma by Nexera HPLC (Japan)
Here, using the AXIMA Microorganism Identification System, consisting of the AXIMA MALDI-TOF MS developed by Shimadzu in conjunction with our database search software for microorganism identification, we introduce the results of our investigation of the identification capability of the MALDI-TOF MS, in discriminating among strains of Escherichia, in which the homology rate of the 16SrRNA gene sequence is greater than 95%.
View here (978221 KB)

Analysis of the Decomposition Products of Lithium Hexafluorophosphate in the Electrolytic Solution of Lithium-Ion Rechargeable Batteries by Column-Switching Ion Chromatography (Part 2)
Lithium hexafluorophosphate is commonly used as the electrolytic solution in lithium-ion rechargeable batteries. It is hydrolyzed by the small amounts of water contained in the electrolytic solution to produce fluoride and other ions. In Application News L417, we presented an example of analysis of electrolytic solution which had deteriorated due to exposure to air, using a column-switching ion chromatography system. Here, we introduce an analysis of an electrolytic solution that had been subjected to accelerated deterioration during testing.
View here (1170319 KB)

HPLC Application - Increasing the Throughput of UHPLC
Mycotoxins are low-molecular-weight natural products produced by fungi and are capable of causing disease and death. Mycotoxins are typically found in grain products and their occurrence is increased under certain heat and humidity conditions. Regulatory levels have been set for mycotoxin levels, and are dependent on the end use of the food products. Mycotoxin levels can vary widely within the same crop, creating a potential need for increased testing to provide more accurate mycotoxin levels. A high-speed UHPLC method was developed that could provide separation of eight common mycotoxins in less than two minutes to allow for increased testing. Details of the method will be presented.
View here (1197407 KB)

LCMS-8030/8040 Application - High Speed Analysis of Mycotoxins (SSI)
In general, the key issue in an optimization procedure for HPLC separation is the selection of the mobile phase and/or column, which is called “Scouting” and has a critical effect on the chromatographic separation. Much time and effort is required for method scouting under conventional HPLC conditions. Meanwhile, Ultra High Performance Liquid Chromatography (UHPLC) has become widely used in recent years, and is expected to be a core technology in the method scouting process in order to reduce labor and cost. In this situation, we have developed a method scouting system based on the Nexera UHPLC system.
View here (924305 KB)

Increasing the Throughput of UHPLC
UHPLC has proven to be an effective way to reduce analysis times without losing separation efficiency through the use of small particle and core-shell column technologies. The use of higher column temperatures and shorter column lengths has allowed the analysis speed of UHPLC to be further increased. A number of high-speed UHPLC applications and conditions will be presented which now allow up to four analytical runs to be completed in only a one-minute timeframe.
View here (1197407 KB)

High Speed Analysis of Mycotoxins
Mycotoxins are low-molecular-weight natural products produced by fungi and are capable of causing disease and death. Mycotoxins are typically found in grain products and their occurrence is increased under certain heat and humidity conditions. Regulatory levels have been set for mycotoxin levels, and are dependent on the end use of the food products. Mycotoxin levels can vary widely within the same crop, creating a potential need for increased testing to provide more accurate mycotoxin levels. A high-speed UHPLC method was developed that could provide separation of eight common mycotoxins in less than two minutes to allow for increased testing. Details of the method will be presented.
View here (924305 KB)

Auto Dilution of Standard and Sample Solutions Using the SIL-30AC Autosampler
Pretreatment operations were shown to require less time and effort when using the automatic dilution feature of the SIL-30AC. Furthermore, these automated functions allow highly accurate results, free of technician-related errors. When using the SIL-30AC, automatic dilution and automatic reagent addition can easily be set up by using standard templates. Also, use of pretreatment programs makes it possible to set up very complex operations for a wide range of functions to be executed automatically.
View here (378640 KB)

Using a Phenyl Column When Separation with C18 (ODS) Is Insufficient
The C18 column is an ODS type of column that is marketed by instrument and column manufacturers, in which octadecyl groups are bonded to a silica base to provide wide separation applicability. An appropriate ODS column is typically the first type selected from the various types available at the start of a reverse-phase analysis. However, in the process of investigating the mobile phase conditions, there are cases in which the separation conditions cannot be improved. Selecting a different ODS column or exchanging it with a C8 column to improve separation is also possible, but even then, it may not be possible to achieve sufficient separation.
View here (304819 KB)

High Speed, High Resolution Analysis (Part 45) Analysis of Pre-Column Derivatized Amino Acids by the Nexera SIL-30AC Autosampler (Part 2)
Here, we introduce an example of the determination of 26 amino acids using a different column size and different mobile phase conditions than were used in L432. The automatic pretreatment feature of the SIL-30AC was utilized for derivatization of the amino acids during analysis, thereby enabling the overall analysis time to be substantially shortened.
View here (1157266 KB)

HPLC Application 3rd party - Clinical Applications for Decade II ECD
This application note describes a Multiple Reaction Monitoring (MRM) method for low-level detection of PCBs in human blood serum using the Shimadzu GCMSTQ8030 triple quadrupole GC/MC/MS. Chromatograms, calibration data, and full operating conditions, including MRM transitions and optimized collision energies, are presented in subsequent tables and figures. Data from five human blood serum samples are included.
View here (1434390 KB)

Cookie Cutter Proteolysis: Achieving Reproducible, Efficient Digestions for Proteomic Workflows
Protein sample preparation workflows for mass spectrometric analysis that involve proteolysis are often labor-intensive, time consuming and user dependent. These workflows often involve digestion, solid phase extraction, drying, and re-suspension prior to reversed phase separation into the mass spectrometer. The introduction of variability at many of these steps hinders discovery initiatives as well as the ability to convert these discoveries into viable assays. Recently, an automated protein digestion platform was developed which accelerates the digestion process through use of immobilized enzyme reaction (IMER) columns. Furthermore, online digestion is integrated with desalting and reversed phase chromatography to create a seamless workflow to the mass spectrometer once the sample is injected. The benefit of streamlining these processes can be demonstrated by the reproducibility achieved.
View here (2796300 KB)

Determination of Drugs in Serum using Heart-cutting Two-dimensional Ultra High Performance Liquid Chromatography
HPLC separation and quantitation are often used for measurement of drug concentrations in the blood. When analyzing the concentration of a drug in blood using HPLC, it is necessary to separate analytes from other compounds. However, the separation of analytes and other compounds in blood is not easy because of the complex matrix. Sample preparation is useful for these cases to reduce matrix, but it can take a long time. In this poster, we analyzed propranolol in serum using heartcutting two-dimensional ultra high performance liquid chromatography. This method was developed on our UHPLC system equipped with a high-pressure switching valve.
View here (834680 KB)

LCMS-8040 Application - Detecting Nucleoside Post Enzymatic Cleavage Modifications in RNA Using Fast Product Ion Scanning Triple Quadrupole Mass Spectrometry (SSI)
Pueraria mirifica [Leguminosae] is a plant species native to Thailand whose tuberous roots are used medicinally for their anti-ageing properties. P. mirifica is a source of several phytoestrogens and flavonoids such as deoxymiroestrol, puerarin, genistein, and many others. Renewed interest in the herb as well as higher standards of identity and purity demand accurate and precise methods for detecting the various compounds in P. mirifica extracts both qualitatively and quantitatively. UHPLC-MS-MS is an effective strategy to characterize such extracts and accurately measure its key components. A selective and sensitive UHPLC-MS-MS method meeting these requirements was developed.
View here (388516 KB)

Fractional Determination of Co-eluted Compounds Using a New Data Processing Method for Photodiode Array Detector
The i-PDeA derivative spectrum chromatogram method was developed as a new data processing technique for photodiode array detectors for HPLC. A derivative spectrum is created by performing differential processing on the UV-Vis absorption spectrum at each measurement time. Plotting the derivative spectrum values at the specified wavelength against retention time creates a derivative spectrum chromatogram that is able to separate co-eluted peaks. The high selectivity of the derivative spectrum chromatogram can detect unexpected impurities and quantitate the target component only, without effects from interfering components that elute simultaneously. This paper formulates the theory of the derivative spectrum chromatogram method into mathematical expressions and reports details of verification of the basic performance using standard samples.
View here (646785 KB)

LCMS-8040 Application - An automatic versatile system integrating solid-phase extraction with ultra-high performance liquid chromatpgraphy-tandem mass spectrometry using dual-dilution strategy for direct analysis of auxins in plant extracts (China)
Here, we tried a comprehensive separation by using a semi-micro reversed-phase column and neutral pH mobile phase for 1st dimension and an ultra-high speed reversed-phase column and acidic pH mobile phase for 2nd dimension. Herbal medicines contain many relatively-polar compounds, so pH is said to be important parameter.
View here (1355832 KB)

Nexera XR UHPLC 3rd Party Application - Efficient Identification of Deoxynivalenol in the Global Wheat Food Chain—Testing Unprocessed, Processed, and Consumer Wheat Products (Horizon)
Five wheat samples with varying degrees of processing were tested for natural levels of deoxynivalenol, as well as spiked for determination of recovery. A recovery comparison of the manual SPE results to the automated SPE results shows that both values meet EU limits; however, the apparent technician bias is revealed as a factor in accurate safety levels reported when the percent recovery difference is compared.
View here (1324138 KB)

Analysis of Impurities in New-generation Antidepressants by Prominence-i
Pharmaceutical companies in Japan are under notification by the Ministry of Health, Labour and Welfare to carefully consider the administration of the new-generation antidepressant drugs that have been on the market since 1999 in Japan to patients under the age of 181). Further, to ensure the properties and suitability of these drugs, they are listed in the United States Pharmacopoeia (USP) and European Pharmacopoeia (EP). The new Prominence-i integrated high-performance liquid chromatograph features separation compatibility with the systems of other companies. Further, use of the delay volume-compatible system kit option provides separation compatibility with the previous LC-2010 model, thereby permitting the smooth transfer of methods from the currently used instrument. Here, using the new Prominence-i integrated high-performance liquid chromatograph, we introduce an example of analysis of compounds related to the abovementioned new-generation antidepressants.
View here (998546 KB)

Comprehensive 2D Separation of Triglycerides in Vegetable Oil with ELSD/LCMS-IT-TOF Detection
Triglycerides, molecules consisting of a glycerol backbone to which three fatty acids are attached via ester bonds, are considered important functional components in both animal oil and vegetable oil. Triglycerides display low solubility in aqueous solvents, and their separation has typically been conducted by either silver ion-mediated normal phase analysis or reversed phase analysis using an organic solvent. However, as there are numerous molecular species consisting of combinations of fatty acids, mutual separation of the triglycerides in natural fats can be difficult using any single set of separation conditions. The Nexera-e comprehensive two-dimensional liquid chromatograph effectively achieves mutual separation of such complex components.
View here (1375265 KB)

LCMS-2020 Application - Evaluation of Current HPLC System Capabilities (SSI)
The use of ultrahigh pressure liquid chromatography (UHPLC) to reduce analytical run times continues to increase in popularity. However, some instrument performance parameters are sometimes sacrificed to allow operation at these high pressures, which are currently approaching 19,000 psi. A recently introduced UHPLC system was evaluated to test instrument performance at ultrahigh pressures. A variety of UHPLC environmental and pharmaceutical applications will be presented to demonstrate the performance that was obtained.
View here (1177031 KB)

SFC/SFE Application - Online Supercritical Fluid Extraction-Supercritical Fluid Chromatography (Online SFE-SFC)
Online supercritical fluid extraction-supercritical fluid chromatography (online SFE-SFC) system is that directly connects the supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC). By using the online SFE-SFC, pretreatment to analysis can be automated, creating advantages such as simplification of pretreatment, analysis of unstable compounds, and high-sensitivity analysis. Here, we introduce the basic principle of online SFE-SFC, the characteristics of the “Nexera UC Online SFE-SFC System,” and examples of extraction analyses.
View here (687418 KB)

i-Series Application - BioEthanol Analyzer - Effect Column Temperature Bioethanol HPLC Part 1
This article looks at the results of a simple study conducted to investigate the effect of different column temperatures on the resulting chromatograms. The ion exclusion form of chromatography commonly used in fermentation monitoring is a combination of several different mechanisms, all of which may be affected by temperature. Increasing column temperature will have an effect on the mobile phase viscosity, but also will increase the kinetic mobility of molecules in solution, thereby enhancing or enabling the occurrence of interactions.
View here (1262281 KB)

Cannabis Analyzer Application News - Potency Testing in Cannabis Extracts Using a High Resolution Method with Cannabis Analyzer
Cannabis may be analyzed for different purposes, the most common of which is the potency, characterized by the quantitation of THC, CBD and CBN. This application note highlights the use of a high resolution HPLC method to determine the potency of cannabis extracts with the Shimadzu Cannabis Analyzer for Potency. With this method, the most commonly requested cannabinoids may be determined in less than 30 minutes with full baseline resolution. Further, the method handles a growing number of cannabinoid targets.
View here (461160 KB)

Cannabis Analyzer Application News - Potency Testing in Cannabis Extracts Using a High Sensitivity Method with Cannabis Analyzer
Cannabis may be analyzed for different purposes, the most common of which is the potency, characterized by the quantitation of THC, CBD and CBN. This application note highlights the use of a high sensitivity HPLC method to determine the potency of cannabis extracts with the Shimadzu Cannabis Analyzer for Potency. With this method, the most commonly requested cannabinoids may be determined in under 10 minutes and with the sharpest chromatographic peaks.
View here (481660 KB)

Cannabis Analyzer Application News - Potency Testing in Cannabis Extracts Using a High Throughput Method with Cannabis Analyzer
Cannabis may be analyzed for different purposes, the most common of which is the potency, characterized by the quantitation of THC, CBD and CBN. This application note highlights the use of a high throughput HPLC method to determine the potency of cannabis extracts with the Shimadzu Cannabis Analyzer for Potency. With this method, the most commonly requested cannabinoids may be determined in under 8 minutes.
View here (450951 KB)

Nexera Application - Ultrafast Analysis of Water-Soluble Vitamins
"Water-soluble vitamins such as thiamine (vitamin B1) and riboflavin (vitamin B2) are generally analyzed by reverse-phase ion-pair chromatography. This document introduces an example of ultrafast analysis performed on water-soluble vitamins by gradient elution using Nexera and a Phenomenex Kinetex C18 column (particle size 2.6 µm, a core-shell column where a 0.35 µm porous membrane is combined with a 1.9 µm solid core). Aflatoxins are mycotoxins with a carcinogenic property and acute toxicity. They are measured by fluorescence detection HPLC and other instruments in order to prevent contamination of foods. Among four components (B1, B2, G1, G2) quantitated as the total aflatoxin, sensitivity for B1 and G1 is generally enhanced by a derivatization process using trifluoroacetic acid. Using the RF- 20Axs High-Sensitivity Fluorescence Detector enables these components to be directly detected at a high sensitivity without any derivatization process. This document introduces an example of ultrafast, high-sensitivity analysis performed on aflatoxins using Nexera and the RF-20Axs."
View here (184821 KB)

A High Sensitivity LC/MS/MS Method with QuEChERS Sample Pre-treatment for Analysis of Afl#31;atoxins in Milk Powder Samples
Afl#31;atoxins (B1, B2, G1 and G2) are metabolites produced by fungi (Aspergillus favus and Aspergillus parasiticus) in crops, animal feed and dairy products. A#31;flatoxins are highly toxic contaminants in food and feed and their amounts increase under bad storage conditions favourite for fungal growth. Afl#31;atoxin M1 is a hydroxylated metabolite of a#31;flatoxin B1 found in milk of cow fed with a diet contaminated with a#31;flatoxin B1[1]. A#31;flatoxin B1 is known the most carcinogenic among all the afl#31;atoxins, and hence its metabolite afl#31;atoxin M1 is given critical attention. Strict regulations for a#31;flatoxin M1 in milk and dairy products have been set. For example, European Union (EU) limits the level of afl#31;atoxin M1 to no more than 0.05 μg/kg in milk and dairy products and 0.025 μg/kg in infant food. We present a high sensitivity LC/MS/MS method for quantitative analysis of the #30;ve a#31;flatoxins (B1, B2, G2, G2 and M1) in milk powder incorporating QuEChERS sample pre-treatment procedure, which is more cost effective as compared to the traditional procedure using immunoaf#30;nity column (IAC)[2]. High sensitivity and good recoveries were achieved using this LC/MS/MS method.
View here (357459 KB)

HPLC Application 3rd party - Advantage of a New Generation of Evaporative Light Scattering Detectors: universaally, Higher Sensitivies and Cost-Effectiveness for multi-Element Analyses in Liquid Chromatography- An Application Review (SEDERE)
Among the detectors available in Liquid Chromatography, Evaporative Light-Scattering Detector (ELSD) became in recent years a well established instrument thanks to several theoretical studies based on fundamental investigations and numerous applications provided during the last thirty years. Indeed, ELSD is considered as a nearly Universal, powerful and cost-effective technique, and is ideally appropriate for the majority of the liquid chromatography applications. Today, the power of this detection mode is further extended with a new model which proposes a genuine and efficient Low-Temperature technology (LTELSDTM) combined with an innovative detection chamber, thus providing the highest sensitivities with all compounds including semi-volatile and thermo-labile ones.
View here (868177 KB)

HPLC Application - High-speed Analysis for Amino Acid Using OPA-FMOC Auto-Precolumn Derivatization with Nexera System
Almost half of the drugs currently used in medical treatments are ionic compounds, which are provided as salts formed with counter-ions. The physicochemical and pharmacokinetic properties of those drugs are influenced by the types of the counter-ions. In the process of drug discovery, the selection of counter-ions is intensively investigated. Ion chromatography (IC) is generally appropriate to analyze inorganic or organic ions but not suitable for drug compound analysis due to its large hydrophobicity. On the other hand, reversed phase liquid chromatography (RPLC) is mainly applied for analysis of drug compounds. Fig. 2 shows chromatograms of pharmaceutical counter-ions obtained by using an ion exchange column. Consequently, it is difficult to analyze a drug compound and its counter-ions simultaneously. To overcome this drawback, we have developed a RPLC x IC system which affords simultaneous and easy determination of pharmaceutical salts.
View here (548029 KB)

New Data Processing Method for Photodiode Array Detector
A new data processing method for a photo diode array (PDA) detector, Intelligent Dynamic Range Extension Calculator (i-DReC) enables the automatic calculation of peak area and height, utilizing spectrum similarity in the high concentration range where UV signal is saturated. When the integrated chromatographic peak area exceeds a user-defined threshold value, i-DReC automatically shifts the chromatographic profile to a wavelength with less UV absorption to prevent signal saturation. The absorption ratio between the original target wavelength and the wavelength used by the i-DReC function is applied as a correction factor to the peak area of the acquired chromatogram, thereby calculating the peak area and height at the original target wavelength. The i-DReC dramatically extends the linear dynamic range of calibration curves, enabling reliable quantitation of high concentration samples without need for sample dilution and reinjection, which would otherwise be required.
View here (582175 KB)

Nexera XR UHPLC 3rd Party Application - Determination of Deoxynivalenol in Shredded Wheat Cereal using Automated Solid Phase Extraction with Immunoaffinity Cartridges (Horizon)
Deoxynivalenol is a common mycotoxin found in agricultural grain crops and final consumer processed products. Most impacted are wheat, barley, and corn. Deoxynivalenol, also known as Vomitoxin, is produced by Fusarium fungi and has a unique dual-stage growth cycle of producing mold during warm daylight and toxin during cool nights. There is no known procedure or processing that will remove deoxynivalenol that is already present in grain. Vomitoxin, has the ability to withstand high processing temperatures, creating the need for food safety determination of both agricultural crops and processed foods prior to consumption by animals and humans. If consumed, the Fusarium mycotoxin produces serious illness and is known for being one of the most endangering on animal and human health. Identifying deoxynivalenol contamination in wheat products quickly, effectively, and with a high degree of confidence relies heavily on the accuracy of laboratory procedures and measurements.
View here (1133432 KB)

Comprehensive two-dimensional HPLC analysis coupled with mass spectrometric detection and informative data processing for lipid analysis
In lipidomics, phospholipids are the attractive targets of analysis since lipids are important and essential components of biological membranes. However, conventional HPLC system by a single separation mode performs poorly on biological lipid sample, because it contains various kinds of lipids with common moieties that govern their behavior on column. In such a case, comprehensive two-dimensional (2D) LC will be a powerful tool. This system was capable of characterizing phospholipids both quantitatively and qualitatively when coupled with triple quadrupole and ion trap-TOF type of mass spectrometer respectively. Reliable identi#31;cation of lipid species was performed by acquiring m/z values of related parent and fragment ions at high accuracy with the ion trap-TOF mass spectrometer and matching the data to commercially available data-base.
View here (597235 KB)

Analysis of Nivalenol and Deoxynivalenol in Wheat Using Prominence-i
Nivalenol and deoxynivalenol (DON, vomitoxin) are types of mycotoxins produced by Fusarium fungi. In Japan, the provisional reference value for deoxynivalenol was set at 1.1 ppm in May, 2002 (Notification No. 0521001 issued by Department of Food Safety, Pharmaceutical and Food Safety Bureau, Ministry of Health, Labour and Welfare of Japan). Previously, in Application News No. L362, the analysis using an ultra high-performance LC system was introduced, but here, referring to the test method for deoxynivalenol specified in the Notification No. 0717001 (issued by Department of Food Safety, Pharmaceutical and Food Safety Bureau, Ministry of Health, Labour and Welfare of Japan, in July 2003), a washing process for the analytical column is included. The detector component of the new Prominence-i integrated high-performance liquid chromatograph incorporates a temperature control function for both the flow cell component and the optical system. Here, good repeatability was obtained despite the susceptibility of UV detection in the short wavelength region due to environmental temperature fluctuations.
View here (108354 KB)

Analysis of Omeprazole by "i-Series" for USP and JP Methods
Omeprazole, a drug that effectively suppresses the excessive secretion of gastric acid, is often used for the treatment of gastric ulcer and duodenal ulcer, in addition to the treatment of reflux esophagitis. Acting as a Proton Pump Inhibitor (PPI), omeprazole is included in the WHO Model List of Essential Medicine, and considered an important component of basic medical care. This Application News introduces an example of analysis of omeprazole in accordance with the Japanese Pharmacopoeia (JP) and the United States Pharmacopeia (USP). Also presented here is an example of analysis that can be completed in a significantly shorter time than that described in the USP General Chapter 621 Chromatography. The Nexera-i integrated UHPLC was used for the analysis by the procedure described in the USP. The Nexera-i supports the use of analytical conditions specified for both HPLC and UHPLC. In the case of compliance (HPLC conditions) with the Japanese Pharmacopoeia, we conducted analysis using the Prominence-i integrated HPLC.
View here (919526 KB)

Automated Optimization of Chiral Separation Parameters Using Nexera UC Chiral Screening System
Chiral compounds contain asymmetric carbons in their molecules and are not superimposable on their mirror images. HPLC has been the main method used to separate such chiral compounds, but in recent years, the use of supercritical fluid chromatography (SFC) has been gaining attention. The main mobile phase used for chiral SFC is supercritical carbon dioxide, with low polarity, low viscosity, and high diffusivity, to which polar organic solvents (modifiers) are added to control solubility and polarity. Therefore, chiral compound separation by HPLC, which generally uses normal phase conditions, offers the potential for high speed, low organic solvent consumption, low cost, and low environmental impact. However, chiral SFC requires selecting a variety of separation parameters, such as columns and modifiers, which can involve large amounts of time and effort. This article describes using the Nexera UC chiral screening system to automatically optimize the large number of separation parameters by switching between up to 12 columns and various mixture ratios of four types of modifiers. This can significantly reduce the effort required.
View here (1576256 KB)

Analysis of Unstable Compounds Using Online SFE-SFC
Supercritical fluids have characteristics of both gas and liquid; low viscosity, high diffusivity and solubility. In particular, carbon dioxide becomes a supercritical fluid at a relatively modest critical point (31.1 °C and 7.38 MPa). Due to its low toxicity, inertness, easy availability, and low cost, supercritical carbon dioxide fluid is used in a wide variety of fields. Analytical applications using it include supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC). Previously SFE and SFC were offline operations for pretreatment or analysis, respectively, and treated as completely separate workflows. However, now SFE and SFC can be connected online using the Nexera UC system, which allows integration of all the processes from pretreatment to data acquisition into a single workflow. This article describes using the Nexera UC system for online SFE-SFC analysis.
View here (1012554 KB)

Using the Nexera UC Online SFE-SFC-MS System to Analyze Residual Pesticides in Agricultural Products
The Nexera UC online SFE-SFC-MS system combines supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC) in one online system, so that the entire process from extraction of target components to acquisition of data can be performed completely automatically. Furthermore, the system can add polar organic solvents (modifiers) to the supercritical carbon dioxide fluid during SFE and SFC, so that the system can be used to extract and analyze components with a wide range of polarities. Meanwhile, ever since the positive list system was enacted in 2006 in Japan for residual pesticides in foods, which applies to more than 800 types of pesticides, there has been increasing demand for a system able to simultaneously analyze multiple pesticides with a wide range of properties, including pretreating samples. This article describes an example of using the Nexera UC online SFE-SFC-MS system to analyze residual pesticides in agricultural products.
View here (2038546 KB)

HPLC 3rd Party Application - Improving Data Reliability and Laboratory Efficiency Testing of Fluoroquinolones in Fatty and Non-Fatty Fish Samples with One Method using Automated Solid Phase Extraction and New Consumable Technologies (Horizon)
The optimized method parameters showed both high fat and low fat fish samples were effectively recovered following LLE and SPE extraction steps. The larger pore and particle size of the Strata-XL-C SPE cartridges in combination with the SmartPrep Extractor System efficiently automated the combined LLE sample extracts to achieve consistent %RSD values across both high and low-fat fish matrices. Using new column technology with the uHPLC system improved peak resolution for increased sensitivity at the specified 20-ppb FDA monitored level. Elution of all four fluoroquinolone peaks occurred in 7 minutes compared to the 20 minutes using the original column technology.
View here (1280684 KB)

HPLC 3rd Pary Application - A Novel Method for Pre-Column Derivatization of Aflatoxin B1, B2, G1, and G2 Prior to HPLC Analysis using the XcelVap® System as a Thermostatically-Controlled Heated Water Chamber (Horizon)
The XcelVap Evaporator/Concentrator System was successfully used to optimize pre-column derivatization of all four aflatoxin standards (B1, B2, G1, G2). The enclosed, dark, and moist heated environment allowed for consistent linearity results to be obtained prior to fluorescence HPLC detection. Elaborate technology and post-column derivatization should not be a requirement for derivatization when common laboratory equipment can be used effectively and at a lower cost. Many journal resources have researched and reported a variety of times and temperatures for performing derivatization; however, for the highest confidence and most efficient quantitation, it is recommended to test a few derivatization times. In this application note, the longer derivatization time produced optimal results. Chromatography was used as an indicator of full derivatization, and peak fronting was been shown to be a reasonable factor in considering whether the derivatization process was complete.
View here (871454 KB)

LabSolutions Application - Data Integrity Compliance Using the LabSolutions Report Set
A recent topic related to analytical data is the lack of data integrity due to data modification and replacement. Whether caused intentionally or accidentally, such problems are often the result of incorrect operating procedures. Accordingly, the question of how to ensure data integrity has become a pressing issue for analysis laboratories. In addition to the sophisticated security functions provided in the previous version, LabSolutions DB/CS version 6.50 includes a new Report Set function that enables the visibility of software operations. Therefore, not only can it help ensure the reliability of the analysis data required by analysis laboratories but, it can also cut decrease the amount of time needed to check analysis results to a half of or a third of that previously required.
View here (441084 KB)

High Speed Analysis of Explosives
Showcasing the development and use of a high-speed reversed phase method for monitoring explosive levels in soil samples near current and former munition plants, an important objective for both environmental and safety reasons.
View here (840789 KB)

Investigation of Synthetic Compounds in Drug Discovery by Nexera-i and LCMS-2020
Here, we introduce an example of analysis of eight pharmaceutical substances in a workflow that is typically used for pharmaceutical synthesis confirmation analysis.
View here (1459556 KB)

Simultaneous Determination of Asulam, Thiophanate- Methyl, Siduron, Iprodione by Prominence-i
Here, simultaneous analysis of these four pesticides in a standard sample was conducted in compliance with the "Separate Method 9" using the Prominence-i integrated high-performance liquid chromatograph, and the measurement accuracy and linearity were then evaluated.
View here (942546 KB)

LCMS-8060 Application - Quantitative analysis of 646 pesticides (1,919 MRMs) by LC-MS/MS with fast 10.5 minute cycle time (SEG)
With an increasing global population, food security is increasingly under threat and there is a growing challenge for agriculture to produce more food, safely and more sustainably. The use of herbicides, insecticides and fungicides reduce crop losses both before and after harvest, and increase crop yields. However, pesticide residues resulting from the use of plant protection products on crops may pose a risk to human health and require a legislative framework to monitor pesticide residues in food. National programs for pesticide monitoring in the US, Europe and Japan have set Maximum Residue Levels (MRL’s) or tolerance information (EPA) for pesticides in food products. A default value of 0.01 mg/kg is applied for MRL enforcement, which therefore requires highly sensitive and specific analytical technologies to monitor an increasing number of pesticides. This paper describes the expanded capability of the LCMS-8060 to help accelerate method development work flows and support increased pesticide monitoring programs. Using the Shimadzu Pesticide MRM Library (the Library includes information on 766 certified reference materials) a single multi-residue LC/MS/MS method was developed for 646 pesticides (typically 3 MRM transitions for each targeted pesticide resulting in 1,919 transitions in total, with a polarity switching time of 5 msec).
View here (652048 KB)

LCMS-IT-TOF Analysis of Amoxicillin
Amoxicillin was successfully separated and detected under gradient conditions using a Shimadzu Prominence series LC coupled to the LCMS-IT-TOF. Data acquired on the LCMS-IT-TOF allows for MSn and excellent mass accuracy within one experiment. Mass accuracy data obtained from the LCMS-IT-TOF is comparable to data reported by other vendors requiring the use of an internal standard or a dual-sprayer configuration.
View here (285 KB)

GC Application - Fast Analysis of Acrylonitrile in ABS Polymer Using a Backflush GC System
Here we introduce an example of high resolution analysis of a BSA (Bovine Serum Albumin) digest*1 using an “LCMS-IT-TOF” combination system consisting of the Prominence UFLCXR ultra fast, high speed LC with the Shim-pack XR-ODS II high speed, high resolution column (particle size 2.2 µm) and an ion trap mass spectrometer (QIT)/time-of-flight mass spectrometer (TOF).
View here (1305746 KB)

[ARCHIVED] Supporting Pharmaceutical Cleaning Validation with TOC and UV-Vis Spectrophotometric Analysis
Analysis of impurities can be a challenging task especially when the main ingredient needs to be assayed at the same time, which requires a wider dynamic range and lower baseline disturbances. With an extra wide dynamic range, temperature-controlled flow cell and a stray-light correction function, both SPD-20A UV and SPD-M20A Photo Diode Array detectors offer a high level of stability, sensitivity and linearity for a confident analysis. The 100 Hz sampling of the SPD-20A/M20A ensures peak information can be captured without loss of resolution and exploits the full potential of ultra-fast LC columns.
View here (423656 KB)

MALDI-Performance Application - On-Tissue MALDI Analysis: Analysis of Spatiotemporal Changes in Energy Metabolism in a Murine Middle-Cerebral Artery Occlusion Model (Japan)
High-speed analysis of preservatives in cosmetics was previously introduced in Application News No. L375, but we have updated this application as an example of ultra-high-speed analysis with the Nexera LC system in conjunction with the Shim-pack XR-ODS III high-speed separation column.
View here (1556754 KB)

Analysis of PFCs in Environmental Water Using Triple Quadrupole LC/MS/MS (LCMS-8030)
Organofuorine compounds such as perfuorooctanoic acid (PFOA) and perfluorooctanesulfonic acid (PFOS) are highly stable chemical compounds which are widely used as water repellents, oil repellents and coating agents. These compounds do not decompose easily in the natural world due to their stability. Reports of their detection in rivers, streams, tap water, food, as well as in the atmosphere and in human blood has led to concern of their effect on the human body as environmental pollutants. Here we conducted the simultaneous analysis of PFOA, PFOS, and related compounds using the LCMS-8030. The results of an environmental water monitoring study that we conducted are also presented.
View here (1428778 KB)

Analysis of Pesticides in Foods Using a Triple Quadrupole LC/MS/MS [LCMS-8030]
Pesticides are widely used in agricultural products to protect crops from insect infestation during cultivation and product transport. With the heightened concern for food safety, “Positive List System” was introduced in Japan on May 29, 2006. These limits ban the sale of food containing pesticides that exceed specified concentrations to ensure the safety of food circulating in the market. Currently, residue standards and analytical methods have been established for about 800 kinds of pesticides and veterinary pharmaceuticals, and this number is expected to increase even further. Therefore, there is increasing need for simpler analytical methods capable of simultaneous multi-residue analysis.Here, using the LCMS-8030, we optimized methods for the simultaneous multi-residue analysis of 43 pesticides, and report the results of the analysis of actual vegetable extracts (paprika and leek) in solution.
View here (981656 KB)

GCMS-TQ8030 Application - Metabolites in Rat Urine Using Scan/MRM via GC/MS/MS (Part 2) (Japan)
Here we report a new on-line SPE-LC-MS/MS method with multiple injection function using an auto-sampler, which enhances not only the throughput, but also the trapping efficiency and recovery of the analysis.
View here (180401 KB)

LCMS-8030/8040 and LCMS-IT-TOF Application - Analysis of Hemoglobin Variants using an Automated Sample Preparation Workstation Coupled to LC-MS (SSI)
The evolution of collision cells for tandem mass spectrometry is influenced by a variety of application needs and includes improved sensitivity, signal to noise and ion-transmission speeds. Ultrafast Mass Spectrometry (UFMS) on triple quadrupole instruments offers the opportunity to simultaneously acquire fragmentation data from a single compound at several different collision energies without compromising the integrity of the peak shape. In this application, we use UFMS to generate data for multiple analytes in a single run using complimentary pathways to improve the certainty of analyte identification.
View here (8938327 KB)

LCMS-8030 Application - Identification of triazolam, etizolam and their metabolites in biological samples by liquid chromatography tandem mass spectrometry (Japan)
Here the quantitative analysis of endogenous H2S level in tissue samples was performed by coupling the monobromobimane-based assay to triple quadrupole LC/MS/MS. Furthermore, this method has an advantage of the measurement at neutral pH to quantify biologically free-gaseous H2S not acid-labile H2S and this approach is expected to be a useful method to quantify free H2S level in tissue samples.
View here (543295 KB)

LCMS-8030/8040 Application - Simultaneous analysis of anionic, amphoteric, and non-ionic surfactants using ultra-high speed LC-MS/MS (Japan)
In this study LCMS technology, developed for ultra-fast scanning MRM analysis, allows the possibility of a single generic ‘universal’ method. High speed MRM analysis and a generic parameters were used for screening 172 pesticides (344 MRM transitions) with 5 msec dwell and 1 msec pause times in food matrices.
View here (113575 KB)

LCMS-8040 Application - Exploring the application of a universal method for pesticide screening in foods using a high data acquisition speed MS/MS (Japan)
In this study, we report the application of ultra-fast 5 msec MRM with 15 msec polarity switching for the analysis of 138 pesticides in vegetable matrices (72 and 66 compounds measured by LC-QqQ and GC-QqQ in the European Union Reference Laboratory (EURL) method) .
View here (353804 KB)

[ARCHIVED] Analysis of Acephate in Water Using GC-MS
Detection of impurities in active pharmaceutical ingredients (APIs) is often conducted using an HPLC-UV method. However, qualitative and quantitative analysis of impurities requires not only the separation of the impurities from the major component, but also separation among impurities themselves. The time and effort required to establish effective analytical conditions for this type of analysis are significant. Furthermore, the source of the impurity, whether it be the sample itself or some external factor associated with a particular lot, must also be determined. Here we demonstrate analysis of an impurity in an API using the 2-dimensional LC/MS/MS separation feature of the Co-Sense for Impurities System.
View here (345601 KB)

GCMS Application - High-Sensitivity Analysis of 2,4,6-Trichloroanisole in Wine Using Headspace-Trap GC/MS (HS-20, Japan)
The European Union Reference Laboratory (EURL) has reported their results on evaluating the validity of residual pesticide analysis utilizing GC-MS/MS and LC-MS/MS1). In their report, the measurement of 66 pesiticides using GC-MS/MS was recommended. This data sheet presents selected results of analysis of these pesticides using the triple quadrupole GCMS-TQ8030.
View here (193218 KB)

GCMS-TQ8040 Application - Automatic Optimization of Transitions and Collision Energies on the GMCS-TQ8040 (Japan)
Pain management is a branch of medicine employing an interdisciplinary approach for easing suffering and improving the quality of life of those living with pain. We herein describe a novel five minute LC-MS/MS assay for quickly identifying and quantifying drugs (a large pain panel) in human plasma. Utilizing ultra fast positive and negative polarity switching with a triple quadrupole mass spectrometer, it is demonstrated that both positive and negative ions from many drug classes in human plasma can be easily quantified in a single injection, with chromatographic peak widths spanning only 3-4 seconds.
View here (312346 KB)

LCMS-8040 Application - Quantitation of Pain Management Drugs Using Ultra-Fast Liquid Chromatography/Mass Spectrometry in Human Plasma Utilizing Positive/Negative Polarity Switching (SSI)
Pain management is a branch of medicine employing an interdisciplinary approach for easing suffering and improving the quality of life of those living with pain. We herein describe a novel five minute LC-MS/MS assay for quickly identifying and quantifying drugs (a large pain panel) in human plasma. Utilizing ultra fast positive and negative polarity switching with a triple quadrupole mass spectrometer, it is demonstrated that both positive and negative ions from many drug classes in human plasma can be easily quantified in a single injection, with chromatographic peak widths spanning only 3-4 seconds.
View here (411279 KB)

LCMS-8050 Application - Application of a Sensitive Liquid Chromatography-Tandem Mass Spectrometric Method to Pharmacokinetic Study of Telbivudine in Humans (China)
This poster employed a liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) method to determinate 16 benzimidazole residues in animal tissue. The method is simple, rapid and high sensitivity, which meets the requirements for the analysis of veterinary drug residue in animal tissue.
View here (151589 KB)

LCMS-8050 Application - Investigation of Instrumental Variables Effect on Intact Protein Multiple Reaction Monitoring Reproducibility in a Next Generation Triple Quadrupole Mass Spectrometer (SSI)
Here, we present a novel 2D-LC/MS/MS method with APCI interface for direct analysis of 1α,25-diOH-VD3 in serum. The method achieved a detection limit of 3.1 pg/mL in spiked serum samples with 100 uL injection.
View here (1058697 KB)

MALDI-iDplus Application - iDplus Reference Publications for MALDI Assurance, Confidence, and Performance
Carboxy THC is an important compound found in marijuana. The Substance Abuse and Mental Health Service Administration (SAMHSA) has set 40% of the cutoff value (15 ng/mL) as the target for the lower limit of quantitation (LLOQ) for carboxy THC. The following Application News will describe a Nexera-8030 LC/MS/MS method for measuring carboxy THC for the LLOQ.
View here (444333 KB)

GCMS-QP2010 Ultra Application - Analysis of Residual Solvents - Class 1, Class 2A, Class 2B - in Pharmaceuticals Using Headspace-GC/MS (Japan)
IGF-1 is a protein that is used in the screening of growth hormone deficiencies, as well as testing for abuse in professional sports. Detection using an LCMS approach is emerging as a preferred test to the standard immunoassay due to the improved reproducibility that LC-MS offers as well as the ability to multiplex and identify biologically relevant changes such as post translational modifications.
View here (1453184 KB)

GCMS-QP2010 SE Application - GCMS-1406 Shimadzu Guide to US EPA Method 624 11172014.pdf
Trenbolone and ethynyl estradiol were optimized on column on the LCMS-8050 triple quadrupole mass spectrometer in APCI positive and negative mode with polarity switching. Gradient LC conditions were applied to detect 50 pg on column with at least a signal to noise (S/N) ratio > 100 for both analytes.
View here (1027111 KB)

"GCMS-QP2010 SE Application - Shimadzu Guide to US EPA Method 624 for Analysis of Volatile Organic Compounds in Wastewater"
This application note describes a GCMS purge-and-trap (P & T) method validation study conducted to evaluate operating conditions for the existing US EPA Method 624 VOC list, using updated technology and advanced GCMS instrumentation. GCMS instrument operating conditions are provided which bring the method in line with capabilities provided by contemporary laboratory equipment. This application note provides calibration results across three different ranges, complete MDL and Precision and Accuracy studies at multiple concentrations, and analysis of an independent laboratory VOC reference standard and real-world samples.
View here (1027111 KB)

LCMS-8050 Application - Quantitative Analysis of Veterinary Drugs Using the Shimadzu LCMS-8050 Triple Quadrupole Mass Spectrometer (Japan)
Due to their low polarity, pyrethoid pesticides are typically measured by GC and GC-MS, however this Application News demonstrates simultaneous positive and negative-ion mode analysis of 14 pyrethroid pesticides using LC-MS/MS with electrospray ionization (ESI).
View here (1471396 KB)

TOC Application - TOC-4200 - TOC Monitoring Upstream of Paper Mill Wastewater Treatment
This Application News introduces examples of high-speed, high-sensitivity analysis of four drug substances, including the endothelin receptor antagonists (ERA) bosentan and ambrisentan, and the phosphodiesterase-5 (PDE-5) inhibitors sildenafil and tadalafil. All of these substances are used as therapeutic agents for the treatment of pulmonary arterial hypertension (PAH), and the analysis was conducted by LC/MS/MS using ESI in positive mode.
View here (1255150 KB)

Quantitative Analysis of Pyrethroids in Soil and Sediment Using the Shimadzu LCMS-8050 Triple Quadrupole Mass Spectrometer
Pyrethroid pesticides are used widely around the world as agricultural and household insecticides. Synthetic pyrethroids are slightly soluble in water and easily adsorbed in soil. In recent years, pyrethroid residues have been confirmed in soil and sediment in both agricultural and urban areas. Pyrethroids, while posing little danger to humans, exhibit a high toxicity to aquatic organisms and insects, making their impact on the ecosystem a matter of concern. Therefore, there is a need for a sensitive technique which can rapidly measure pyrethroid pesticides in soil and sediment. Due to their low polarity, pyrethroid pesticides are typically measured by GC and GC-MS, however this Application News demonstrates simultaneous positiveand negative-ion mode analysis of 14 pyrethroid pesticides using LC-MS/MS with electrospray ionization (ESI).
View here (1027546 KB)

Comprehensive Monitoring Method for Analyzing 158 Lipid Mediator Species Using the Ultra-Fast LCMS-8050
Lipid mediator is a generic term for bioactive lipids, which are produced in the body and play a role in many biological functions. Simultaneous analysis of over 100 lipid mediatorrelated compounds has recently been developed by achievement of high speed and high sensitivity on a comprehensive LC/MS system. Comprehensive monitoring of the lipid mediators resulted in showing a causal relationship between lipid mediators and various disorders. A lot of isomers of lipid mediator species show the same molecular weight and MS/MS spectrum, therefore chromatographic separation is needed for identification. “LC/MS/MS Method Package for Lipid Mediator Ver. 2” was developed to simultaneously analyze 158 lipid mediator-related compounds by ultra-fast triple quadrupole mass spectrometry. This application data sheet presents a list of targets and an example for measuring lipid mediators in various biological tissues. Furthermore, 87 arachidonic acids and its metabolites, 18 EPA and its metabolites, 16 DHA and its metabolites, 11 ethanolamids, 23 metabolites of other fatty acids, Azelaoyl-PAF, PAF and Lyso-PAF are all included as registered compounds in the method in order to analyze a total of 158 components with optimized MRM transitions and retention times. Lipid mediator is a generic term for bioactive lipids, which are produced in the body and play a role in many biological functions. Simultaneous analysis of over 100 lipid mediatorrelated compounds has recently been developed by achievement of high speed and high sensitivity on a comprehensive LC/MS system. Comprehensive monitoring of the lipid mediators resulted in showing a causal relationship between lipid mediators and various disorders. A lot of isomers of lipid mediator species show the same molecular weight and MS/MS spectrum, therefore chromatographic separation is needed for identification. “LC/MS/MS Method Package for Lipid Mediator Ver. 2” was developed to simultaneously analyze 158 lipid mediator-related compounds by ultra-fast triple quadrupole mass spectrometry. This application data sheet presents a list of targets and an example for measuring lipid mediators in various biological tissues. Furthermore, 87 arachidonic acids and its metabolites, 18 EPA and its metabolites, 16 DHA and its metabolites, 11 ethanolamids, 23 metabolites of other fatty acids, Azelaoyl-PAF, PAF and Lyso-PAF are all included as registered compounds in the method in order to analyze a total of 158 components with optimized MRM transitions and retention times.
View here (979155 KB)

Simultaneous Analysis of Culture Supernatant of Mammalian Cells Using Triple Quadrupole LC/MS/MS
Industrial fermentation for the production of biofuels or biopharmaceutics requires routine monitoring of medium conditions such as pH, dissolved gas, carbon source (glucose) and nitrogen source (glutamine) for optimization and control of the fermentation process. However, culture media also consist of various other biologically important compounds such as vitamins, nucleic acids and other primary metabolites, which would lead to more detailed understanding of the bioprocess if monitored altogether. To meet the demand for comprehensive analysis of medium component, we optimized the analytical conditions and developed this “Method Package for Cell Culture Profiling” that can monitor relative abundance of 95 compounds listed herein. Using this Method Package, we demonstrated the change in abundance of culture medium components associated with hybridoma growth over a period of 5 days.
View here (885546 KB)

High-Sensitivity Determination of Catecholamines in Plasma Using the LCMS-8060 Triple Quadrupole LC/MS/MS
Catecholamines are a family of signaling molecules found in brain, adrenal medulla and other nervous systems. Catecholamines i n plasma, namely norepinephrine (NE), epinephrine (EP) and dopamine (DA), are commonly measured in clinical research. Analysis of catecholamines in plasma requires both high sensitivity and high throughput. Presented here is a platform designed to demonstrate the capability to detect catecholamines in plasma, comprising multiplexed plasma sample preparation by Biotage EVOLUTE WCX solid phase extraction followed by high-sensitivity quantitation by LCMS-8060.
View here (922654 KB)

Rapid Analysis of Immuno-suppressants Using Triple Quadrupole LC-MS/MS
This report exemplifies an ultra high speed analysis of 4 immuno-supressants (Tacrolimus, Everolimus, Rapamycin, Cyclosporin A) in less than 120 seconds by Shimadzu UFMS Triple Quadrupole Mass Spectrometer LCMS-8050 with negative ionization mode. Combination of Nexera X2 and LCMS-8050 provides you much faster run time than ever you experienced without sacrificing the quality of results.
View here (608754 KB)

LCMS-8040 Application - High-Throughput Optimization of Therapeutic Drug Monitoring Using Fully Automated Sample Preparation LCMSMS System (CLAM-2000 + LCMS-8040) (Japan)
This article introduces the results of TDM using a fully automated sample preparation LC/MS/MS system comprised of the CLAM-2000 fully automated LCMS sample preparation unit and the LCMS-8040 high performance liquid chromatograph-mass spectrometer. This system resolves the above-mentioned problems associated with TDM, and achieves TDM research results on a fast and high-precision analytical workflow.
View here (1880210 KB)

LCMS-8060 Application - High-Sensitivity, High-Throughput Quantitation of Catecholamines and Metabolites in Plasma by Automated WCX-SPE Coupled to LC/MS/MS for Clinical Research (Japan)
Catecholamine levels in plasma, namely norepinephrine (NE), epinephrine (E) and dopamine (DA), give indication of disease states and are routinely measured for clinical research. Recently, plasma catecholamine metabolites such as metanephrine (MN) and normetanephrine (NMN) are increasingly studied as an alternative of or to complement catecholamine levels. Therefore high-sensitivity and high-throughput analytical system that covers all of these compounds is warranted. We herein demonstrate our optimized LCMS method for simultaneous determination of plasma NE, E, DA, MN and NMN in plasma and evaluated its performance with respect to a predicate device.
View here (639691 KB)

LCMS-8060 Application - LC/MS/MS High Sensitivity Bioanalytical Method: Entecavir in Human Plasma (Asia Pacific)
Here we describe a simple, fast and high sensitivity bioanalytical method for quantitative determination of entecavir in human plasma on Shimadzu LCMS-8060 system with a heated ESI and coupled with UHPLC. The high sensitivity and robust interface design of the system allow the use of protein-precipitation only in plasma pre-treatment and achieve a LLOQ of 40 pg/mL in plasma or 10 pg/mL in the injection solution after pre-treatment of plasma sample with 1uL injection volume.
View here (392499 KB)

LCMS-8060 Application- Enhanced Sensitivity for Assay of Sulfonamide Drugs and Trimethoprim in Honey by LCMS Triple Quadrupole Mass Spectrometry with QuEChERS Extraction (SSI)
Twenty one sulfonamides along with trimethoprim were analyzed by LC-MS/MS using a Nexera HPLC system coupled to an LCMS-8060 triple quadrupole mass spectrometer. Diverse clean up sorbents for extraction and purification were tested using a QueChERS method.
View here (1373071 KB)

LCMS-8050 Application - LCMS-MS Method for Evaluation of PPCPs in Enviormental Water (SSI)
Pharmaceutical and personal care products (PPCPs) encompass a family of compounds used by individuals for health and cosmetic purposes, as well as compounds used by the agricultural industry to maintain health of livestock. The number of individuals who are using these products is increasing which has caused an increase in environmental detection. The effect on humans and the environment is still unknown causing the need for more research on the topic. These contaminates are introduced into local waterways via sewage plants and natural disposal (ie; animal excrement and landfill waste). This poster demonstrates a method for evaluating PPCPs at parts per billion levels in local waterways using liquid chromatography tandem mass spectrometry (LC-MS/MS).
View here (2430935 KB)

LCMS-8050 Application - Determination of Wilfordine and Wilforine in honey using Liquid Chromatography with Tandem Mass Spectrometry (SSI)
In this paper, a fast and effective method for the sensitive and reliable analysis of Wilfordine and Wilforine using LC-MS/MS was established.The method has good linearity, with correlation coef cient greater than 0.999, the limit of detection were 1.3 and 4.3 ng/mL, the quantification limits were 2.7 and 9.0 ng/L, respectively. The recoveries were between 98.8~116.0%.
View here (414656 KB)

LCMS-8060 Application - High-sensitivity, high-throughput quantitaion of catecholamines and metanephrine in plasma by automated WCX-SPE coupled to LC/MS/MS for clincal research (Japan)
Catecholamine levels in plasma, namely norepinephrine (NE), epinephrine (E) and dopamine (DA), give indication of disease states and are routinely measured for clinical research. Recently, plasma catecholamine metabolites such as metanephrine (MN) and normetanephrine (NMN) are increasingly studied as an alternative of or to complement catecholamine levels. Therefore high-sensitivity and high-throughput analytical system that covers all of these compounds is warranted.
View here (462549 KB)

LCMS-8060 Application - Simultaneous analysis of 23 mycotoxins using ultra-high speed LC-MS/MS with a pentafluorophenyl column (Japan)
Mycotoxins may contaminate food and feed and are known to give serious damages to health of human and animals. For food safety, manufacturers should monitor their products to avoid contamination based on analytical data. Several mycotoxins are regulated in US, EU and JP. The number of mycotoxins regulated continued to increase yearly. Current mycotoxins monitoring methodologies tend to focus on a specific mycotoxins, so it takes a long time to monitor various mycotoxins. In our previous study, we have developed the simultaneous analysis of 14 mycotoxins. This time, we tried to enhance the number of analytical mycotoxins (23 mycotoxins). As carryover of fumonisins (FMs) was observed in the high sensitivity analysis, the minimization of carryover also was attempted.
View here (580277 KB)

High-Speed Analysis of Itraconazole in Plasma Using Triple Quadrupole LC/MS/MS (LCMS-8050)
Itraconazole is a triazole antifungal agent that is used widely for the treatment of infections by fungi including the genera Trichophyton, Aspergillus and Candida. This article introduces an example of high-speed analysis of itraconazole and its active metabolite hydroxy itraconazole in plasma using the LCMS-8050 high-sensitivity triple quadrupole mass spectrometer. Although a simple method of sample pretreatment was used that involves only deproteinization, the quantitative results obtained were excellent in terms of accuracy and precision.
View here (945235 KB)

LCMS-8060 Application - Expanding Capabilities in Multi-Residue Pesticide Analysis Using the LCMS-8060
This application note describes the expanded capability of the LCMS-8060 to help accelerate method development workflows and support increased pesticide monitoring programs. Using the Shimadzu Pesticide MRM Library (the Library includes information on 766 certified reference materials) a single multiresidue LC/MS/MS method was developed for 646 pesticides (3 MRM transitions for over 99 % targeted pesticides resulting in 1,919 transitions in total, with a polarity switching time of 5 msec).
View here (1411526 KB)

Determination of Wilfordine and Wilforine in honey using Liquid Chromatography with Tandem Mass Spectrometry
Tripterygium wilfordii, which contains a lot of biological toxic compounds such as Wilfordine and Wilforine, is one of the toxic nectar plants. The Wilfordine and Wilforine may be transferred to honey by honey bees. Due to the low content and complex matrix, determination of Wilfordine and Wilforine in honey is not easy. In this study, a highly sensitive method based on liquid-liquid extraction (LLE) and LC-MS/MS has been developed. The results showed that the detection limits of Wilfordine and Wilforine in honey sample were 5.16 and 10.80 ng/kg, respectively.
View here (405256 KB)

LCMS-8040/8050 Application - Application of Metabolomics to Microbial Breeding (Japan)
Metabolomics presents useful tools for the evaluation of metabolic changes during microorganism breeding, and for understanding metabolic changes related to a target material and its precursors and intermediates. By deepening our understanding of the metabolic pathways involved in material production, metabolomics is expected to result in more efficient materials production. In this article, we discuss an example of LC/MS analysis of how the sulfur-containing metabolites vary during culture of a cysteine-producing Escherichia coli (E. coli) when either thiosulfuric acid or sulfuric acid is added as the sulphur source during cysteine synthesis.
View here (821993 KB)

LCMS-8050 Application - Analysis of Formaldehyde in Drinking Water Using Triple Quadrupole LC/MS/MS (Japan)
Formaldehyde is highly toxic and the levels are regulated in many products, including cosmetics, textiles, household products, and indoor (work) environments since it is also one of the causes of sick house syndrome. Japan has a water quality standard in place for formaldehyde levels in drinking water (0.08 mg/L), and a test method is specified in appended table 19, solvent extraction-derivatization-gas chromatography-mass spectrometry method, of the methods determined by the Minister of Health, Labour and Welfare based on prescriptions of ministerial ordinance concerning water standards (Health, Labour and Welfare Ministry notification No. 261 of July 22, 2003). Revisions to the ministerial ordinance concerning water.
View here (77562 KB)

LCMS-8050 Application - Analysis of Iminoctadine, Paraquat, and Diquat in Tap Water Using Triple Quadrupole LC/MS/MS (Japan)
Iminoctadine is used as an antimicrobial agent, and paraquat and diquat are used as non-selective herbicides. By the director of Water Supply Division, Health Service Bureau, Ministry of Health, Labour and Welfare (0325 No. 3 to 6) in March 2015, a notification of simultaneous analysis using solid-phase extractionliquid chromatograph-mass spectrometer" (appendix method 21) was issued as a method for testing the presence of these three pesticides in tap water. This article describes an example of analysis of iminoctadine, paraquat, and diquat performed according to appendix method 21. Also described is an investigation into a simplified method that omits part of the sample pretreatment process.
View here (86873 KB)

Efficient extraction of residual pesticides in agricultural products and soils for GC/MS and LC/MS analysis using supercritical fluid extractionon
A solvent extraction is commonly used for pretreatment of residual pesticides in foods and soils. In the method, a substantial amount of time and effort are required and large quantities of organic solvents are consumed. Supercritical fluid extraction (SFE) that employs supercritical carbon dioxide as an extraction solvent provides good extraction efficiency due to high diffusivity and solubility. It affords extremely short time as well as less damaging to the environment due to small consumption of organic solvent compared to that of solvent extraction methods. We have developed an efficient SFE system that can perform up to 48 automatic and serial extractions and applied it to extraction of residual pesticides in agricultural products and soils.
View here (1401253 KB)

LCMS-8060 Application - Determination of Selected ASTM Perfluorinated Compounds (PFCs) Using the Shimadzu LCMS-8060 (SSI)
ASTM methods D7968-14 and D7979-15 are used to determine the same list of PFCs but in different matrices. ASTM method D7968-14 lists soil as a matrix while ASTM method 7979-15 lists water, sludge, influent, effluent and waste water as matrix options. These methods use different extraction techniques but both evaluate the samples by liquid chromatography/tandem mass spectrometry (LC/MS/MS). We evaluated the instrumental portion of the methods using the Shimadzu LCMS-8060 triple quadrupole mass spectrometer. Calibration ranges and estimated detection limits were well within method specified values.
View here (744613 KB)

Analysis of Iminoctadine, Paraquat, and Diquat in Tap Water Using Triple Quadrupole LC/MS/MS [LCMS-8050]
Iminoctadine is used as an antimicrobial agent, and paraquat and diquat are used as non-selective herbicides. By the director of Water Supply Division, Health Service Bureau, Ministry of Health, Labour and Welfare (0325 No. 3 to 6) in March 2015, a notification of "simultaneous analysis using solid-phase extractionliquid chromatograph-mass spectrometer" (appendix method 21) was issued as a method for testing the presence of these three pesticides in tap water. This article describes an example of analysis of iminoctadine, paraquat, and diquat performed according to appendix method 21. Also described is an investigation into a simplified method that omits part of the sample pretreatment process.
View here (85659 KB)

Multi-Residue Analysis of 18 Regulated Mycotoxins by LC/MS/MS
Mycotoxins are one of the most important contaminants in food and feed due to their widespread distribution in the environment and toxic effects on humans and animals.1) Structurally, mycotoxins are a very diverse group with a wide range of physicochemical properties and low molecular weights.2) They are produced by fungi (mould) frequently found on agricultural produce, and are often not visible to the naked eye.3) Some of the most commonly contaminated food stuffs include wheat, oats, rye, corn, barley, rice, nuts and milk.
View here (75365 KB)

LCMS-8060 Application - Phospholipid characterization by a TQ-MS data based identification scheme
Phospholipids play a wide variety of roles such as the structural units of the cellular membrane, the storage and transport of lipids, the precursor of the lipid mediators and the energy source in vivo. To deeply understand the biological function of phospholipids, quantitative analysis for the phospholipid composition ratio in the blood and tissues is required. Phospholipids species have many types of combination of its characteristic head groups and fatty acid composition. Although identification of phospholipid species typically is performed for the data acquired by a high resolution mass spectrometer, in this study, we report phospholipids database search and quantitative analysis by coupling LC-TQ MS with SimLipid software.
View here (641386 KB)

High-Sensitivity Quantitative Analysis of Trace-Level Impurities and Active Ingredients with HPLC
As the trend toward smaller and smaller analyte concentrations progresses, conventional analytical methods are becoming less and less able to address trace-level analyses. For example, not only do product impurities affect product quality, there are increasing instances of product safety being compromised as well. This has prompted increasingly stringent impurity control across a wide range of business enterprises, where concern about quantitative analysis of extremely low levels of impurities is the current reality. On the other hand, when the analyte is the active ingredient itself, it becomes increasingly difficult to establish a quantitative method as the concentrations decrease to minute levels. While the typical approach to addressing this situation is to increase sensitivity by taking such measures as increasing the sample concentration, there is always the concern that the solubility of the principal ingredient may be adversely affected, or that the analyte might not be sufficiently separated from possibly large numbers of obstructing substances in the sample matrix (see Fig. 1). Addressing this situation often necessitates the use of pretreatment procedures such as extraction and concentration, which also adversely affects efficiency due to the extra time and labor involved in conducting complicated pretreatment procedures. Thus, it becomes necessary to satisfy two very different requirements for the quantitation of trace-levels of analytes: increasing measurement sensitivity and speeding up operations. The key point in achieving this is to automate the entire process from the fraction collection (fractionation) and concentration of the analytes to final quantitation.
View here (831900 KB)

HPLC 3rd Party Application - A Unique and Simple Matrix Preparation Roadmap for Aflatoxin B1, B2, G1, G2 Food Safety Testing Prior to Automated SmartPrep® Extractor Solid Phase Extraction (Horizon)
Data demonstrated that one sample preparation method, accounting for matrix moisture, is a viable and reliable solution for a wide range of matrices varying in viscosity and moisture content. The single sample preparation extraction formula developed for LLE followed by automated SmartPrep Extractor SPE with Supel™ Tox AflaZea cartridges using four matrices of almond milk, fresh corn, peanut paste, and curry powder generated acceptable recoveries and %RSD values for sample matrix spikes. Derivatization using the XcelVap offered a consistent moist and dark environment, and in combination with the efficiency of the uHPLC system and column technology, sharp aflatoxin peaks at the lower EU spike levels were generated and easily quantified. Better resolution of the four aflatoxin peaks from any matrix peaks was obtained for high moisture matrices, with sufficient peak height generated by the gradient to quantitate low moisture matrices, as demonstrated by the low %RSD. Using a single sample preparation method for multiple sample matrices reduces error associated with referencing several methods and preparation procedures.
View here (1163451 KB)

SFC/SFE Application - Improved Sample Pretreatment Using Offline Supercritical Fluid Extraction
Separation analysis using HPLC, SFC or GC requires a pretreatment step to ef ciently extract a target constituent from the sample in various forms (e.g., solid). Constituents are usually extracted from solid samples using dissolution or solid-liquid extraction methods. Dissolution methods can only be used when the sample is soluble in a given solvent, and they are dif cult to optimize depending on the analytical conditions. Solid-liquid extraction methods (e.g., Soxhlet extraction) are not suited to the pretreatment of multiple samples as they require considerable time for extraction and non-extraction (e.g., cleaning, preparation) operations. However, extraction methods involving supercritical uids can utilize the characteristics of supercritical uids (e.g., high solubility, permeability) to achieve the elution of a target constituent from a solid sample with high ef ciency and also allow automation during the extraction process. This article describes the utilization of the Nexera UC SFE pretreatment system, which increases the ef ciency of sample pretreatment for analysis.
View here (829600 KB)

GPC-MALDI Analysis of Trace Components in Synthetic Polymers
Matrix-Assisted Laser Desorption / Ionization Time-of-Flight mass spectrometry (MALDI-TOF MS) is being employed in a growing number of synthetic polymer applications in recent years. Using this technique, monomer and terminal structures are predicted based on the masses of the observed polymer substance, molecular weight distribution is evaluated, and molecular structural analysis is conducted by MS/MS analysis.
View here (864999 KB)

Flash and Continuous Light Sources in Fluorescence
For fluorescence measurements from the ultraviolet through the visible and into the near infrared region, the typical light source is the Xenon arc lamp. This particular source has been widely used due to its favorable characteristics, primarily the ability to deliver high energy output over a wide wavelength range.
View here (366735 KB)

Analysis of Cortisone Acetate Tablets by Nexera UC SFC System
This application note shows an example of the analysis of cortisone acetate tablets according to the USP monograph. The original normal phase method was transferred to an SFC method with a conventional column, Shim-pack CLC-SIL, then a highspeed column, Shim-pack XR-SIL by using the Nexera UC SFC system.
View here (349523 KB)

Analysis of Polystyrene with Antioxidant Additive Using Prominence-i GPC System
The new Prominence-i integrated high-performance liquid chromatograph supports connection with the RID-20A differential refractive index detector. In addition, as the column oven can house up to three 30 cm columns used for GPC analysis, applications that require a long column are also supported. Here, we introduce an example of GPC analysis of polystyrene using the Prominence-i GPC system.
View here (978545 KB)

Analysis of Omeprazole by "i-Series" for USP and JP Methods
The Nexera-i integrated UHPLC was used for the analysis by the procedure described in the USP. The Nexera-i supports the use of analytical conditions specified for both HPLC and UHPLC. In the case of compliance (HPLC conditions) with the Japanese Pharmacopoeia, we conducted analysis using the Prominence-i integrated HPLC.
View here (915456 KB)

Automatically extraction and analysis using on-line supercritical fluid extraction (SFE) / supercritical fluid chromatography (SFC) system
The online SFE-SFC-MS system is capable of user-friendly simultaneous multicomponent analysis, with online automation of everything from sample pretreatment to separation and analysis. It will be of practical use in fields where faster and more reliable automatic analysis of multiple samples is required, such as in the examination of residual pesticides in foods, and searches for disease biomarkers.
View here (848545 KB)

Analysis of Malachite Green Using a Triple Quadrupole LC/MS/MS [LCMS-8030]
Malachite green, besides being used as a dye in the textile and paper industries in Japan, is also used as a synthetic antibacterial drug to treat diseases such as water mold disease in aquarium fish. Due to concern related to its carcinogenicity and genotoxicity, not to mention the persistence of its metabolite, leucomalachite green, application of malachite green with aquaculture animals is prohibited under the Pharmaceutical Affairs Act. The United States in 1981, and the European Union and China in 2002 prohibited its use with all food-related items. However, due to its low price, effectiveness, and easy availability, cases of its detection in eel, salmon and other farmed fish continue to appear, resulting in strengthened worldwide monitoring.Here, we show the quantitative analysis of malachite green and leucomalachite green using the LCMS-8030.In addition, we report the results of spiked-recovery measurements conducted using a salmon extract solution as an actual sample.
View here (796762 KB)

LCMS-8030/8040 Application - Accelerate method development using fast screening of mobile phases additives and solvents for optimum sensitivity in LC-MS (France)
The main anti-cancer drugs used in cancer chemotherapy can be classified into several categories: cytotoxic, the most represented, but also hormones, immune response modifiers and antibodies. Most cytotoxic agents used in cancer chemotherapy interact with DNA or its precursors. Very few studies are evaluating the future of these drugs in wastewater. Potential risks associated with these discharges are poorly understood and require study work and research to better understand the hazards, exposure characterization and assessment risks to human health and the environment. The purpose of the study is to establish an analytical methodology to screen most of the anti-cancer drugs currently used in hospital waste waters
View here (65554 KB)

LCMS-2020 Application - Quantitative Analysis of Carbohydrates and Artificial Sweetners in Food Samples using GFC-MS with APCI Interface and Post Column Reagent Addition (Asia Pacific)
Non-targeted metabolomics entails data exploration to find the important metabolites from the detected features. Liquid chromatography mass spectrometry (LC-MS) is frequently used for non-targeted metabolomics because of the analytical sensitivity for a wide variety of compounds. In non-targeted metabolomics, compound identification is an important step to translate the information obtained from the instrument such as retention time and m/z into biologically relevant information such as chemical name and structure. We therefore developed a compound identification technique with scoring using both prediction formulae and assignment of product ions for narrowing the candidates. Using this approach, each candidate is evaluated not only using partial structural information from the spectral assignment, but also using all the molecular information provided by formula prediction.
View here (114400 KB)

LCMS-8040 Application - Determination of 68 Veterinary Drugs in Marine Products by Ultra High Performance Liquid Chromatography/Triple Quadrupole Mass Spectrometry (China)
Pesticides are widely used in crop planting and growth process. However, residual pesticides in food could enter human body and harm to human health. Therefore, the maximally allowed residual pesticides in food have strictly regulated in the world. In recent years, the China government continues to strengthen supervision and is developing quicker and highly sensitive analytical method. Usually, the qualitative LC/MS/MS is based on the ratio of intensities between targetions and reference ions. But in some special occasions, especially for determination of low concentration samples, qualitative reliability is not high enough, which may cause false positive/negative results. So use of MS/MS library for screening and qualitative confirmation of the unknown pesticides is very meaningful. This paper describes UHPLC/MS/MS, a rapid and accurate screening method for determination of 200 residual pesticides in agricultural products.
View here (92737 KB)

LCMS-8050 Application - Simultaneous Quantitative Analysis of 20 amino acids in Food Samples without Derivatization using LC-MS/MS (Japan)
Chili powder is one such complex matrix that can exhibit matrix effect (either ion suppression or enhancement). A calibration curve based on matrix matched standards can demonstrate true sensitivity of analyte in presence of matrix. Therefore, this approach was used to obtain more reliable and accurate data as compared to quantitation against neat (solvent) standards[1]. Multiresidue, trace level analysis in complex matrices is challenging and tedious. Feature of automatic MRM optimization in LCMS-8040 makes method development process less tedious. In addition, the lowest dwell time and pause time along with ultra fast polarity switching (UFswitching) enables accurate, reliable and high sensitive quantitation. UFsweeperTM II technology in the system ensures least crosstalk, which is very crucial for multiresidue pesticide analysis.
View here (603017 KB)

LCMS-8040 Application - High Sensitivity Quantitation Method of Dicyandiamide and Melamine in Milk Powders by Liquid Chromatography Tandem Mass Spectrometry (Asia Pacific)
The objective of this study is to develop a fast LC/MS/MS method for direct analysis of amphetamines in urine without sample pre-treatment (except dilution with water) on LCMS-8040, a triple quadrupole system featured as ultra fast mass spectrometry (UFMS). The compounds studied include amphetamines (AMPH), methamphetamine (MAMP) and three newly added MDMA, MDA and MDEA by the new SAMHSA guidelines, four potential interferences as well as PMPA as a control reference. Very small injection volumes of 0.1uL to 1uL was adopted in this study, which enabled the method suitable for direct injection of untreated urine samples without causing signi cant contamination to the ESI interface.
View here (178216 KB)

LCMS-8050 and IT-TOF Application - Comprehensive Two-Dimensional HPLC Analysis Coupled with Mass Spectrometric Detection and Informative Data Processing for Lipid Analysis (Japan)
A cerebral oxidation stress makes them induce insomnia and etc. So, it is desirable to take antioxidants with high penetration through blood-brain barrier (BBB) for the prevention of insomnia. We had found a new antioxidant, 3,5-dihydroxy-4-methoxybenzyl alcohol (E6), from a soft-body extract of Crassostrea gigas, which has antioxidation ability about 2.4 times more than that of alpha-tocopherol and L-ascorbic acid and then we synthesized and identified E6. This time, we developed the method to analyze E6 sensitively by LC-MS/MS and we veri ed the penetrating ability through blood-brain barrier of E6.
View here (610751 KB)

LCMS-8050 Application - High Sensitivity Analysis of Diarrhetic Shellfish Poisoning (DSP) Toxins Using Liquid Chromatography Tandem Mass Spectrometry (Japan)
In lipidomics, phospholipids are the attractive targets of analysis since lipids are important and essential components of biological membranes. However, conventional HPLC system by a single separation mode performs poorly on biological lipid sample, because it contains various kinds of lipids with common moieties that govern their behavior on column. In such a case, comprehensive two-dimensional (2D) LC will be a powerful tool. This system was capable of characterizing phospholipids both quantitatively and qualitatively when coupled with triple quadrupole and ion trap-TOF type of mass spectrometer respectively. Reliable identification of lipid species was performed by acquiring m/z values of related parent and fragment ions at high accuracy with the ion trap-TOF mass spectrometer and matching the data to commercially available data-base.
View here (961656 KB)

LCMS-8050/8060 Application - Multi-Residue Analysis of Pesticides in Crude Food Extracts Using a Sample Extraction Technique and LC/MS/MS (Japan)
Analysis of pesticide residues in food is typically tedious and time-consuming due to the necessary extraction and clean up procedures. Furthermore, to deal with the ever-growing number of pesticides, the food safety laboratories need to ideally screen as many compounds as possible in a single run which may reach maximum residual limits (MRL); typically 10 ppb in food matrices. In this study, we illustrate the results utilizing an UF MRM capability (just 5 msec. MRM measurement includes dwell and pause time) with 5 msec. polarity switching (UF switching) for the analysis of 146 pesticides in crude food extracts by using easy and simple sample preparation technique.
View here (1003831 KB)

LCMS-8060 Application - Rapid Method Development for Targeted LC-MS Screening and Quantification of Proteins from Complex Biological Matrices Using a Retention Time Library in Place of Protein Standards (SSI- MSACL)
QQQ is a robust platform for quantifying targeted proteins from complex biological samples. Typically, quantitative protein assays are developed using comparable synthetic or expressed peptide/protein standards to first establish method conditions. This process can be time consuming and expensive. The method described here does not use authentic protein standards instead, the proteins of interest are targeted and quantified using MRM methods developed from Skyline-software. The identity of the targeted protein is established by the retention time and the sequence specific fragment ions. An UHPLC method specific Retention Time-library created from the tryptic-digest of a mixture of readily available proteins was used to accurately predict retention times. Here, we demonstrate the method’s validity and its application to plasma proteins from a chicken-model of inflammation.
View here (1998198 KB)

LCMS-8050 Application - Determination of Oleanolicacid and Ursolic acid in loquat leaf extract By Liquid Chromatography-Tandem Mass Spectrometry (China)
Ursolic acid (UA) and oleanolic acid (OA) belong to a class of triterpenic acid, which play signi cant bioactive roles in anti-in ammatory, antitumor as well as enhancing the cellular immune system. However, due to the lack of suitable chromophoric or ionization groups in molecular structures, both UV and MS responses are far from satisfaction. In this study, a highly sensitive method based on derivatization and LC-MS/MS has been developed. After being extracted, a pair of stable isotope probes, 2-dimethylaminoethylamine (DMED) and d4-2-dimethylaminoethylamine (d4-DMED) were added for derivatization. The generated heavy labeled triterpenic acids were used as internal standards for quantification, the detection sensitivities of analytes improved sharply, the detection limits of OA and UA were 0.92 and 1.06 ng/L, respectively.
View here (358222 KB)

LCMS-8060 Application - Efficient extraction of residual pesticides in agricultural products and soild for GC/MS and LC/MS analysis using supercritical fluid extraction (Japan)
A solvent extraction is commonly used for pretreatment of residual pesticides in foods and soils. In the method, a substantial amount of time and effort are required and large quantities of organic solvents are consumed. Supercritical uid extraction (SFE) that employs supercritical carbon dioxide as an extraction solvent provides good extraction ef ciency due to high diffusivity and solubility. It affords extremely short time as well as less damaging to the environment due to small consumption of organic solvent compared to that of solvent extraction methods. We have developed an efficient SFE system that can perform up to 48 automatic and serial extractions and applied it to extraction of residual pesticides in agricultural products and soils.
View here (1434146 KB)

LCMS-8050 Application - Simultaneous analysis of supernatant components of cell culture using truple quadrupole LC/MS/MS (China)
Fermentation for the production of biofuels, biopharmaceutics or other compounds requires routine monitoring of medium conditions such as pH, dissolved gas, carbon source and nitrogen source for optimization and control of the fermentation process. However, culture media also consist of various other biologically important compounds such as vitamins, nucleic acids and other primary metabolites, which would lead to more detailed understanding of the bioprocess if monitored altogether. To meet the demand for comprehensive analysis of medium components, we optimized analytical conditions and developed “Method Package for Cell Culture Profiling” for monitoring relative abundance of 95 compounds. Using this method package, we demonstrated the change in abundance of culture supernatant (bacteria and streptomyces cells) components for over the culture periods.
View here (965714 KB)

LCMS-8060 Application - Toxicological General Unknown Screening (GUS) by triple quadrupole LCMS/MS with high sensitivity product ion scan library indentification (SEG)
Forensic toxicological sample measurement can take two paths commonly referred to as targeted and untargeted analysis. Targeted approaches on triple quadrupole platforms are well established with MRM/SRM detection and quantitation for pre-determined lists of compounds. For untargeted analysis, general unknown screening (GUS) acquires full scan MS data to trigger MS/MS spectra at a broad range of collision energies above a predefined threshold. This work describes the application of a nominal mass library acquired with certified reference materials to screen and identify forensic toxicology samples in a routine clinical laboratory. The LC-MS/MS method was designed to acquire MRM and scanning data with polarity switching in a single data le. The MRM data was used to provide quantitative results on commonly encountered target compounds and full scan data to help confirm identification.
View here (159205 KB)

LCMS-8040 Application - Rapid development of quantitative method for determination of plant growth regulators and streptomycin in fruits using LC/MS/MS (India)
Plant growth regulators (PGRs) and antibiotics are commonly used by farmers for enhancing growth of crops and to protect against infections respectively. However, extensive usages of these compounds is known to have adverse effect on human health. Each standard has different linearity range. It is challenging to quickly develop multi-analyte quantitation method for determination of varied compounds simultaneously. One interesting approach can be Method Scouting, which allows user to conduct all method development exercises automatically. This results in swift development of an optimum method which will suit all analytes. Highly sensitive quantitative method was developed quickly using Nexera Method Scouting system for determination of eight PGRs and streptomycin (shown in Figure 1) on LCMS-8040 (shown in Figure 2), a triple quadrupole mass spectrometer from Shimadzu Corporation, Japan.
View here (1504570 KB)

LCMS-8060 Application - Highly sensitive multiplexed analysis of Levosalbutamol from plasma using LC/MS/MS (India)
Salbutamol is the most widely used short-acting  β2-agonist in the symptomatic relief of asthma and Chronic Obstructive Pulmonary Disease (COPD). In all formulations, salbutamol consists of a racemic mixture of equal amounts (50:50) of (R)- and (S)- isomers. Although these isomers are chemically identical, they differ in conformation, being exact non-superimposable (mirror) images of one another, or stereoisomers. (R)-salbutamol has been shown to have a 2-fold greater binding affinity than racemic albutamol and a 100-fold greater binding affinity than (S)-salbutamol for the β2-adrenergic receptor. As a result, the bronchodilator property of racemic (R,S)-salbutamol is attributed entirely to (R)-salbutamol which is also known as ‘Levosalbutamol’. There is an increased demand by pharmaceutical organizations to quantitatively estimate levosalbutamol at lower levels due to reduced dosages for paediatric formulations. With this increase in demand, there is a necessity to increase the throughput of highly sensitive levosalbutamol analysis.
View here (550969 KB)

LCMS-8050 Application - Development of MRM-based detection of the plant metabolome using liquid chromatography/tandem mass spectrometry (Japan)
Multiplexed metabolite screen using MRM-MS has become a powerful strategy to bring information of biological state. In the field of plant research, it is hoped that the metabolomics is used for developing new varieties of plants to get a valuable feature, for understanding for the stress-response from environmental conditions and so on. Liquid chromatography-mass spectrometry is one of a widely used tool for metabolome analysis, and it have an advantage of widely applicable properties, to analyze high molecular weight, thermolabile and polar compounds without any derivatization. In this study, we attempted to develop a LC-MRM-based approach to determine metabolite profiles including both primary and secondary metabolites aiming at high throughput and comprehensive methods using triple quadrupole MS acquisition.
View here (615682 KB)

LCMS-8060 Application - Improved sensitivity for characterization of sulfonamides and trimethoprim in honey using QuEChERS extracts with LC-MS/MS (SSI)
A natural food as honey is subject of diverse restrictions for contaminants presence as the case of antibiotics including sulfonamides. It is a worldwide practice by Beekeepers to use antibiotics as therapeutic agents to treat bee bacterial brood diseases, however the use of sulfonamides (SA) and trimethoprim (TMP) in beekeeping practice is prohibited in EU. There are no a worldwide MRL’s for sulfonamides in honey in the EU, but a minimum required performance level (MRPL) was set for analytical methods at a level of 10 µg/kg of sulfonamides, encouraging the development of reliable laboratory methods for detection in diverse foods included honey. SAs and TMP posing threats to public health causing allergic reactions and increasing microorganism’s drug resistance. Considering MRLs and MRPL of SAs and TMP in food products from animals tend to be continually reduced to preserve human health safety, HPLC-MS/MS is an effective strategy to characterize and accurately measure those antibiotics. The present method is selective, fast, and very sensitive for 20 sulfonamides and trimethoprim.
View here (2043339 KB)

LCMS-8050 Application - Simultaneous Analysis of Culture Supernatant of Mammalian Cells Using Triple Quadrupole LC/MS/MS (Japan)
Industrial fermentation for the production of biofuels or biopharmaceutics requires routine monitoring of medium conditions such as pH, dissolved gas, carbon source (glucose) and nitrogen source (glutamine) for optimization and control of the fermentation process. However, culture media also consist of various other biologically important compounds such as vitamins, nucleic acids and other primary metabolites, which would lead to more detailed understanding of the bioprocess if monitored altogether. To meet the demand for comprehensive analysis of medium component, we optimized the analytical conditions and developed this “Method Package for Cell Culture Profiling” that can monitor relative abundance of 95 compounds listed herein. Using this Method Package, we demonstrated the change in abundance of culture medium components associated with hybridoma growth over a period of 5 days.
View here (383754 KB)

Rapid development of quantitative method for determination of plant growth regulators and streptomycin in fruits using LC/MS/MS
Plant growth regulators (PGRs) and antibiotics are commonly used by farmers for enhancing growth of crops and to protect against infections respectively. However, extensive usages of these compounds is known to have adverse effect on human health [1],[2]. Each standard has different linearity range as shown in Table 2. It is challenging to quickly develop multi-analyte quantitation method for determination of varied compounds simultaneously. One interesting approach can be Method Scouting, which allows user to conduct all method development exercises automatically. This results in swift development of an optimum method which will suit all analytes. Highly sensitive quantitative method was developed quickly using Nexera Method Scouting system for determination of eight PGRs and streptomycin on LCMS-8040, a triple quadrupole mass spectrometer from Shimadzu Corporation, Japan.
View here (1470258 KB)

Determination of Oleanolic acid and Ursolic acid in loquat leaf extract By Liquid Chromatography-Tandem Mass Spectrometry
Ursolic acid (UA) and oleanolic acid (OA) belong to a class of triterpenic acid, which play signi#31;cant bioactive roles in anti-in#30;ammatory, antitumor as well as enhancing the cellular immune system. However, due to the lack of suitable chromophoric or ionization groups in molecular structures, both UV and MS responses are far from satisfaction. In this study, a highly sensitive method based on derivatization and LC-MS/MS has been developed. After being extracted, a pair of stable isotope probes, 2-dimethylaminoethylamine (DMED) and d4-2-dimethylaminoethylamine (d4-DMED) were added for derivatization. The generated heavy labeled triterpenic acids were used as internal standards for quanti#31;cation, the detection sensitivities of analytes improved sharply, the detection limits of OA and UA were 0.92 and 1.06 ng/L, respectively
View here (350125 KB)

Improved sensitivity for characterization of sulfonamides and trimethoprim in honey using QuEChERS extracts with LC-MS/MS
A natural food as honey is subject of diverse restrictions for contaminants presence as the case of antibiotics including sulfonamides. It is a worldwide practice by Beekeepers to use antibiotics as therapeutic agents to treat bee bacterial brood diseases, however the use of sulfonamides (SA) and trimethoprim (TMP) in beekeeping practice is prohibited in EU. There are no a worldwide MRL’s for sulfonamides in honey in the EU, but a minimum required performance level (MRPL) was set for analytical methods at a level of 10 µg/kg of sulfonamides, encouraging the development of reliable laboratory methods for detection in diverse foods included honey. SAs and TMP posing threats to public health causing allergic reactions and increasing microorganism’s drug resistance. Considering MRLs and MRPL of SAs and TMP in food products from animals tend to be continually reduced to preserve human health safety, HPLC-MS/MS is an effective strategy to characterize and accurately measure those antibiotics. The present method is selective, fast, and very sensitive for 20 sulfonamides and trimethoprim.
View here (1996546 KB)

LCMS-8050/8060 Application - Multi-residue analysis of pesticides in crude food extracts using a simple extraction technique and LC/MS/MS
Analysis of pesticide residues in food is typically tedious and time-consuming due to the necessary extraction and clean up procedures. Furthermore, to deal with the ever-growing number of pesticides, the food safety laboratories need to ideally screen as many compounds as possible in a single run which may reach maximum residual limits (MRL); typically 10 ppb in food matrices. In this study, we illustrate the results utilizing an UF MRM capability (just 5 msec. MRM measurement includes dwell and pause time) with 5 msec. polarity switching (UF switching) for the analysis of 146 pesticides in crude food extracts by using easy and simple sample preparation technique.
View here (952365 KB)

LCMS-8050 Application - Measurement of Enzymatic Activities in Dried Blood Spots with On-Line Solid Phase Extraction-LC/MS/MS System (Japan)
Lysosomes are a type of intracellular organelle that uses a variety of hydrolytic enzymes to digest waste matter. To measure the enzymatic activity of lysosomes, methods using artificial fluorescent dyes and tandem mass spectrometry are used. Of these methods, tandem mass spectrometry offers the advantage of being able to measure multiple enzymatic activities at the same time. In this example, a protocol developed at the Meyer Children's Hospital, Mass Spectrometry, Clinical Chemistry and Pharmacology Laboratory (Florence, Italy) was used to measure the enzymatic activity in dried blood spots (DBS) using an online solid phase extraction (SPE) - liquid chromatograph - tandem mass spectrometer (LCMS-8050) system. Because using this system results in samples being cleaned up during SPE, samples can be inserted directly for measurement after enzymatic reaction, without any pretreatment processes.
View here (102082 KB)

LCMS-8060 Application - Ultra-Sensitive and Rapid Assay of Neonicotinoids, Fipronil and Some Metabolites in Honey by UHPLC-LC/MS/MS (Japan)
Neonicotinoids are a class of insecticides widely used to protect fields as well as fruits and vegetables. Recently the use of these compounds became very controversial as they were pointed as one cause of the honeybees colony collapse disorder. Since pollination is essential for agriculture, extensive studies have been conducted to evaluate the impact of neonicotinoids on bee health. Following this the European Food Security Authoritiy (EFSA) limited the use of thiamethoxam, clothianidin and imidacloprid. Fipronil, a pesticide from a different chemical class, has been also banned by EFSA for maize seed treatment due to its high risk for honeybee health. In order to better understand the effect of these compounds on bees and their contamination in pollen and honey, a highly sensitive assay method was necessary. A method was set up using Nexera X2 with LCMS-8060.
View here (642711 KB)

LCMS-8060 Application - Highly sensitive multiplexed analysis of Levosalbutamol from plasma using LC/MS/MS
Salbutamol is the most widely used short-acting β2-agonist in the symptomatic relief of asthma and Chronic Obstructive Pulmonary Disease (COPD). In all formulations, salbutamol consists of a racemic mixture of equal amounts (50:50) of (R)- and (S)-isomers. Although these isomers are chemically identical, they differ in conformation, being exact non-superimposable (mirror) images of one another, or stereoisomers. (R)-salbutamol has been shown to have a 2-fold greater binding af#30;nity than racemic salbutamol and a 100-fold greater binding af#30;nity than (S)-salbutamol for the β2-adrenergic receptor. As a result, the bronchodilator property of racemic (R,S)-salbutamol is attributed entirely to (R)-salbutamol which is also known as ‘Levosalbutamol’. There is an increased demand by pharmaceutical organizations to quantitatively estimate levosalbutamol at lower levels due to reduced dosages for paediatric formulations. With this increase in demand, there is a necessity to increase the throughput of highly sensitive levosalbutamol analysis.
View here (539256 KB)

Measurement of Enzymatic Activities in Dried Blood Spots with On-Line Solid Phase Extraction-LC/MS/MS System
Lysosomes are a type of intracellular organelle that uses a variety of hydrolytic enzymes to digest waste matter. To measure the enzymatic activity of lysosomes, methods using artificial fluorescent dyes and tandem mass spectrometry are used. Of these methods, tandem mass spectrometry offers the advantage of being able to measure multiple enzymatic activities at the same time. In this example, a protocol developed at the Meyer Children's Hospital, Mass Spectrometry, Clinical Chemistry and Pharmacology Laboratory (Florence, Italy) was used to measure the enzymatic activity in dried blood spots (DBS) using an online solid phase extraction (SPE) - liquid chromatograph - tandem mass spectrometer (LCMS-8050) system. Because using this system results in samples being cleaned up during SPE, samples can be inserted directly for measurement after enzymatic reaction, without any pretreatment processes.
View here (100111 KB)

LCMS-8050/8060 Application - Simultaneous Analysis of Tyrosine Kinase Inhibitors in Human Blood Plasma with LC/MS/MS (Japan)
Cancer treatment in recent years employs drugs known as molecular targeted drugs that were developed to target molecules related to the growth, invasion, and metastasis of tumor cells in order to inhibit tumor cell growth. Lung cancer treatment employs tyrosine kinase inhibitors (TKIs), which target the epidermal growth factor receptor (EGFR) and anaplastic lymphoma kinase (ALK), and new molecular targeted drugs, referred to as second and third generation drugs, continue to be developed. This article introduces an example of simultaneous analysis of EGFR-TKIs, ALK-TKIs, and metabolites in human blood plasma for the purpose of research into pharmacokinetics using the triple quadrupole high performance liquid chromatograph mass spectrometer LCMS-8050.
View here (686616 KB)

LCMS-8060 Application - A Highly Sensitive MRM-Based Method for Detection and Quantitation of Seven Pharmaceuticals and Personal Care Products (PPCPs) in Surface Water (Japan)
The presence of pharmaceutical and personal care products (PPCPs) in drinking water has become a growing public concern due to their continuous input and persistence to the environment. They include many drug compounds from medicines and chemical ingredients from daily personal care products such as soaps, toothpastes and cosmetics. Many PPCPs act as endocrine disruptors and thus altering the normal functions of hormones resulting in reproductive defects and health issues. In this Application News, a highly-sensitive LC/MS/MS method is described, which has been developed on a high sensitivity model of triple quadrupole LCMS-8060, aiming at direct determination of seven PPCPs of low ppt levels in surface water samples like treated water and reservoir water without pre-concentration.
View here (670423 KB)

LCMS-8060 Application - Fully automated derivatization - quantification of Glyphosate and AMPA in beer using a standard UHPLC-MS/MS system
Glyphosate is currently one of the most common pesticides used worldwide. In spite of its approval by regulatory bodies all over the world, the concern about its harm to humans and the environment persists. Therefore, the strict control of Glyphosate and its metabolite Aminomethylphosphonic acid (AMPA) in food and environment is mandatory. The chromatography of glyphosate is challenging due to its high polarity. In order to overcome this, there exists a well-established method including a derivatization step with 9-fluorenylmethyl chloroformate (FMOC) followed by LCMS analysis. Here we report a fully automated derivatization followed by LC-MS/MS analysis of beer samples. The instrumental set-up does not require any additional hardware for sample pretreatment but uses the built-in pretreatment function of the autosampler.
View here (156760 KB)

LCMS-8060 Application - Multi-residue veterinary drug analysis of >200 compounds using MRM Spectrum Mode by LC-MS/MS
Veterinary drugs are used for therapeutic, metaphylactic, prophylactic and growth promotion purposes. To provide an assurance that food from animals is safe with regards to residues of veterinary medicines, regulatory authorities have established Maximum Residue Limits (MRL’s) for certain drugs in target tissues and animal species and has also identified pharmacologically active compounds that are prohibited and considered a hazard at any level (EU regulation EC 37/2010; Commission Decision 2003/181/EC; 21CFR Part 556 Tolerances for Residues of New Animal Drugs in Food). In this work, we describe a method that delivers highly sensitive and selective triple quadrupole detection together with MRM Spectrum mode to reduce false positive and false negative reporting. MRM Spectrum mode acquires a high number of fragment ion transitions for each target compound generating a fragmentation spectra that could be used in routine library searching and compound verification using reference library match scores.
View here (2198543 KB)

Analysis of Polymer Additives in Synthetic Polymers using a SEC-MALDI System
Synthetic polymers may deteriorate as a result of various factors such as light, heat, mechanical stress, electrical stress, radiation, chemicals and moisture. Various additives such as antioxidants, UV absorbent, HALS and thermal stabilizers have been developed to maintain the properties of polymers and prevent degradation. The amount of additive depends on the intended use of the polymer but, typically, it is less than 1% (w/w). Analysis of additives in synthetic polymers is therefore important for the evaluation of improvement of polymer properties. Recently, MALDI-TOF MS has been used for the analysis of polymer additives.
View here (753547 KB)

Agent Report: Limiting Report Creation Risks Through Automatic Integration of Various Types of Data
This report entails how to limit report creation risks through automatic integration of various types of data. This report covers ensuring reliability of computer-acquired data, risks to analysis and test data, data alteration, difficulty of handling different types of data, integrating different types of data with agent report, ensuring a high level of security and agent report flexibility and extendibility.
View here (1072213 KB)

Analysis of Anionic Surfactants by Prominence-i and RF-20Axs Fluorescence Detector
According to the Ministerial Ordinance on Water Quality Standards1), an HPLC method using a fluorescence detector has been adopted as the test method for anionic surfactants2). (Please refer to Application News No. L303.) Since either the RF-20A or RF-20Axs fluorescence detector can be connected to the new Prominence-i integrated high-performance liquid chromatograph, the combination of integrated operability and high-sensitivity fluorescence detection is possible. Here we present an example of the analysis of five anionic surfactants using the Prominence-i integrated highperformance liquid chromatograph with the RF-20Axs high-sensitivity fluorescence detector.
View here (1156235 KB)

Analysis of Quasi-Drug by Nexera-i (Part 1) High-Speed, High-Resolution Analysis of Active Ingredient and Preservatives
Quasi-drugs (cosmetics, etc.), in many cases, consist of Table 1 Analytical Conditions an active ingredient together with various components such as preservatives. Typically, a UV detector or photodiode array detector (PDA) is used to conduct qualitative and quantitative analysis of these substances. In particular, a PDA permits qualitative analysis of a UV absorption spectrum and quantitative analysis based on a chromatogram. Following are examples of analysis of the active ingredient in a quasi-drug (cosmetic), in addition to analysis of the coexisting preservatives, using the new Nexera-i integrated ultra-high-performance liquid chromatograph.
View here (949552 KB)

High Speed with High Resolution Analysis by Nexera-I Analysis of Cephem Antibiotics
Cephem antibiotics are a subgroup of β-lactam antibiotics which can be administered orally or by injection similar to the penicillin and carbapenem subgroups. Cephem antibiotics exhibit both a low frequency and low degree of side effects while maintaining a high degree of safety, and can therefore be applied in a wide range of cases. Application News No. L348 introduced an example of high-speed, high-resolution analysis of cephem antibiotics using the Prominence UFLC ultra-fast HPLC system. Here, we introduce an example of high-speed, high-resolution analysis of cephem antibiotics using the new Nexera-i ultra-high-performance integrated liquid chromatograph with a PDA detector.
View here (1090225 KB)

A novel approach to cleaning validation for pharmaceutical manufacturing by online supercritical fluid extraction/supercritical fluid chromatography
Cleaning validation is necessary to establish the quality and safety of pharmaceutical drug products. In cleaning validation protocols, direct sampling is performed with swabs, which are sticks with textiles at one end. The sample on the swab after swabbing the surface of equipment is analyzed with a TOC analyzer and HPLC. Recently, HPLC has been more preferable because of the growing need for the individual analysis of products. Before the HPLC analysis, manual processes such as a sample extraction and a sample condensation are required. Such manual processes may affect to the quality of results. Thus, we evaluated the application of a novel on-line supercritical fluid extraction/chromatography system for the cleaning validation.
View here (1344568 KB)

Analysis of Sugars in Orange Juice and Grape Juice by Prominence-i and Differential Refractive Index Detector
As sugars display little ultraviolet absorption, a differential refractive index detector or an evaporative light scattering detector is used for their detection. The new Prominence-i integrated high-performance liquid chromatograph can be connected to the RID-10A differential refractive index detector. Since the column oven can accommodate a 30-cm column for use in sugar analysis (ligand exchange column), and the temperature can be controlled up to 85 °C, it therefore supports applications that require a long column and high column temperature. Here, we introduce an example of sugar analysis in juices using the Prominence-i with the RID-10A.
View here (1009546 KB)

Peptide Mapping of Antibody Drugs by Nexera-i
Peptide mapping by HPLC is one of the important quality assurance tests used for verifying the primary structure of antibody drugs. Typically, following enzymatic digestion of the antibodies, separation is conducted using a traditional reversed phase column. Due to the large number of peaks that require separation, the use of small-particle columns and core shell columns for peptide analysis has spread in recent years. In order to compare elution profiles for identity and mutation confirmation, a highly repeatable system is required. The Nexera-i integrated UHPLC is the ideal system for such an analysis. Here, the Nexera-i is used in the analysis of IgG (human immunoglobulin G) tryptic digest.
View here (1048545 KB)

A novel approach to cleaning validation for pharmaceutical manufacturing by online supercritical fluid extraction/supercritical fluid chromatography
Cleaning validation is necessary to establish the quality and safety of pharmaceutical drug products. In cleaning validation protocols, direct sampling is performed with swabs, which are sticks with textiles at one end. The sample on the swab after swabbing the surface of equipment is analyzed with a TOC analyzer and HPLC. Recently, HPLC has been more preferable because of the growing need for the individual analysis of products. Before the HPLC analysis, manual processes such as a sample extraction and a sample condensation are required. Such manual processes may affect to the quality of results. Thus, we evaluated the application of a novel on-line supercritical fluid extraction/chromatography system for the cleaning validation.
View here (766545 KB)

Improving the Analysis of Phenylurea Herbicides in Drinking Water and Soft Drinks using Automated Solid Phase Extraction as a Preparation for HPLC-UV Analysis
The application of phenylurea herbicides is very important to increase yields of agriculture products, such as wheat, fruits and cotton. These compounds also have non-agricultural uses as well, such as preservatives in paints. However, the phenylurea herbicides, especially diuron, have been listed by U.S. Environmental Protection Agency as “known/likely” carcinogens. These herbicides are very water soluble and mobile in soils, which leads to contamination of surface water, ground water and eventually drinking water.
View here (1250325 KB)

Analysis of Ions in Drugs (Part 5) Analysis of Organic Acid Counterions by Ion Exclusion Chromatography
Application News No. L457 described an example analysis of chloride, formic acid, acetic acid, and trifluoroacetic acid ions present in drugs using ion chromatography. As mentioned above, drugs can contain multiple different counterions and it is sometimes difficult to separate completely the peaks of these ions using ion chromatography. We describe an example analysis that uses ion exclusion chromatography to increase separation selectivity for formic acid, acetic acid, fumaric acid, and maleic acid, which are organic acids frequently used for drug counterions.
View here (756256 KB)

Cannabis Testing Laboratory Solutions
When purchasing analytical equipment, it is important to know that you are not just buying an instrument but investing in your lab’s future. Shimadzu not only provides the instrumentation but also the technical knowledge and support to help your lab be successful. We can assist with method development, instrument training, and many other areas of support like maintenance to ensure your systems are constantly operating at an exceptional level. From seed to sale, from accurate cannabis potency profi les to reliable, highly sensitive pesticide screening, let us deliver scalable, turnkey solutions to meet your testing needs for today and tomorrow.
View here (8517546 KB)

Assay of Aflatoxin M1 in Milk Based on Notification Test Methodology, Using Prominence-i and the RF-20AXS Fluorescence Detector
Aflatoxin M1 (AFM1) is a mycotoxin suspected of carcinogenicity in humans that is detected in the milk of mammals that eat food contaminated with aflatoxin B1. The notification "Handling of Aflatoxin M1 in Milk" issued on July 23, 2015 (Notification No. 0723-[1] of the Department of Food Safety, PFSB, MHLW) 1) sets a regulatory level for AFM1 in milk of 0.5 μg/kg, and came into force on January 23, 2016. The assay methodology for AFM1 in milk was included in "Test Methodology for Aflatoxin M1 in Milk" (Notification No. 0723-[5] of the Department of Food Safety, PFSB, MHLW) 2) , which was announced on the same day and describes two test methodologies.
View here (794564 KB)

Development of An UHPLC Method for Simultaneous Determination of Thirteen Bisphenols in Milk Samples
An UHPLC method with using a high sensitivity fluorescence detector was developed for fast, well-separation and high sensitivity analysis of thirteen bisphenols, including the most concerned BPA, BPF, BADGE and BFDGE, in milk samples. This new method shows high sensitivity to low μg/L levels, high accuracy and excellent repeatability. The method was applied to spiked milk samples and the results indicated the good feasibility, high sensitivity and reliability in simultaneous determination of thirteen bisphenols in milk samples.
View here (462569 KB)

Fast and High Sensitivity Analysis of Six Preservatives in Beverages by UHPLC with Photodiode Array Detection
In this Application News, a new rapid and high sensitivity UHPLC method for simultaneous determination of the six preservatives in beverages is described. A gradient elution was optimized for separation and quantitation of the six preservatives with a photodiode array detector. A capillary flow cell with extra long optical path of 85 mm was employed to achieve high sensitivity for a very small injection amount of sample (1mL) which was not cleaned up except filtration.
View here (340568 KB)

Comprehensive 2D Separation of Lipid Species in Mussels Using the Nexera-e System Combined with LCMS-IT-TOF Detection
This article presents an example separation of lipids in mussels using the Nexera-e, which is an effective system for the comprehensive separation of a large number of lipid molecules. A semi-micro-scale separation via the HILIC column was used for the first dimension, and an ultra-high-speed reversed-phase separation was used for the second dimension. An ion trap time-of-flight mass spectrometer (LCMS-IT-TOF) was combined with the Nexera-e to perform detection.
View here (1019568 KB)

Simultaneous Determination of Polycyclic Aromatic Hydrocarbons Using the Prominence-i Integrated High Performance Liquid Chromatograph
Many polycyclic aromatic hydrocarbons exhibit fluorescence, and can therefore be detected with high selectivity and high sensitivity using a fluorescence detector. Previously, in Application News No. 393 and No. 441A, we introduced examples of the simultaneous analysis of polycyclic aromatic hydrocarbons (PAHs) using a fluorescence detector. However, of the sixteen polycyclic aromatic hydrocarbons designated as "priority pollutants" by the U.S. Environmental Protection Agency (EPA), acenaphthylene alone does not exhibit f luorescence. Therefore, a s ingle fluorescence detector cannot be used for simultaneous analysis of all sixteen of these PAHs. However, the Prominence-i, which incorporates a UV detector, can be connected to the RF-20Axs fluorescence detector as an optional detector, permitting simultaneous analysis of all sixteen polycyclic aromatic hydrocarbons. Here, using two analytical methods, one with the wavelength switching mode and the other using simultaneous measurement at multiple wavelengths, we introduce an example of simultaneous analysis of the 16 PAHs.
View here (953554 KB)

Analysis of Organic Acids in Culture Medium Using Post-Column pH Buffering Organic Acid Analysis System
Ion-exclusion chromatography using an acidic aqueous solution is used for the separation of the organic acids, but when using an electrical conductivity detector to monitor changes in ion quantities, high-sensitivity detection is difficult due to increased background noise originating from the mobile phase and suppression of the dissociation of the organic acids. With the system mentioned here, after separation of the organic acids by the column, the mobile phase pH is adjusted to nearneutral by mixing with buffer, thus improving detection sensitivity due to dissociation of the organic acids. Previously, an example of improved organic acid separation was described in Application News No. L442, in which two columns were used to achieve better separation than the incomplete separation obtained with a single column. This method offers better separation of organic acids for use in bioproduction, thereby permitting more accurate qualitative and quantitative analysis.
View here (889454 KB)

Improving the Consistency and Accuracy of Tetracyclines Regulatory Laboratory Testing of Contaminated Beef, Chicken, and Cow's Milk with Simple Automation and New Consumables Technology
Tetracyclines are one of the most commonly used antibiotic agents in the United States. A majority of the usage is for agricultural purposes, where it is estimated 80% of tetracyclines administered is for disease prevention in healthy animals. They are also used in farming to keep animals raised in close proximity healthy and gaining weight. In 2012, the FDA indicated, tetracycline accounted for 41 percent of the 31 million pounds of antibiotics sold for farm animals in the United States. While the use of tetracyclines is very beneficial for the production of agriculture products, there are concern about long term adverse health effects for humans. Evidence has shown repeated exposure to low levels of tetracyclines through food sources has lead to antibiotic resistant pathogens. Antibiotic resistance to one drug may transfer to another, especially those within the same drug class. Also, repeated exposure to antibiotics could cause the development of allergies to these compounds, especially in children.
View here (1438545 KB)

Analysis of Polysorbate 80 in IgG Aqueous Solution by Online SPE Using Shim-pack MAYI Column – Part 1 Analysis of Polysorbate 80 in IgG Aqueous Solution by Online SPE Using Shim-pack MAYI Column – Part 1
Various analyses are required in the evaluation of drugs. When analyzing samples that contain macromolecular proteins at high concentrations by reversed phase HPLC, degradation of the column packing is a concern when using a typical ODS column, therefore requiring prior removal of proteins. As the Shim-pack MAYI series, with its packing pore outer surface coated with a hydrophilic polymer, offers a line-up of online SPE columns that can quickly eliminate proteins, when combined with a column switching HPLC, a variety of components can be analyzed in a seamless flow from deproteinization to analysis. Examples of applications related to analysis of drugs in plasma and serum using the MAYI series have previously been reported in Application News No. L285, 286, 293, 305, 307, 315 and 327. By using the Co-Sense for BA bio-sample analysis system, even higher sensitivity, higher precision measurement can be achieved. Here, we introduce an example of analysis of the polysorbate 80 surfactant, widely used as an additive to prevent protein aggregation and adsorption, and to increase protein solubility in a protein formulation.
View here (1204325 KB)

Improving Data Reliability and Laboratory Efficiency Testing of Fluoroquinolones in Fatty and Non-Fatty Fish Samples with One Method using Automated Solid Phase Extraction and New Consumable Technologies
The optimized method parameters showed both high fat and low fat fish samples were effectively recovered following LLE and SPE extraction steps. The larger pore and particle size of the Strata-XL-C SPE cartridges in combination with the SmartPrep Extractor System efficiently automated the combined LLE sample extracts to achieve consistent %RSD values across both high and low-fat fish matrices. Using new column technology with the uHPLC system improved peak resolution for increased sensitivity at the specified 20-ppb FDA monitored level. Elution of all four fluoroquinolone peaks occurred in 7 minutes compared to the 20 minutes using the original column technology .The optimized method passed all FDA criteria for % recovery, % RSD and linearity within less chromatographic time and using current automation and consumable technology. Data presented concludes that while the four fluoroquinolones are structurally similar and exhibit zwitterionic properties, using current consumable chemistries improved overall method efficiency and effectiveness. Improving on work flow by implementing automation for the SPE process with the SmartPrep Extractor enabled objective sample handling across all samples by reducing scientist bias. This improved the reliability of results and the ability to transfer the method to multiple sites for similar results.
View here (125156 KB)

A Unique and Simple Matrix Preparation Roadmap for Aflatoxin B1, B2, G1, G2 Food Safety Testing Prior to Automated SmartPrep® Extractor Solid Phase Extraction
Mycotoxin testing awareness has increased as countries involved in world trade of raw agriculture and processed consumer products rely on a safe global food supply. Several mycotoxins are naturally produced and monitored; however, aflatoxins, produced mainly by the Aspergillus species, are considered to be the most important mycotoxin group in the world’s food supply to monitor1. The frequency of occurrence and negative health impacts to both animals and humans has spiked interest in the aflatoxins B1, B2, G1, and G2 levels present within foods commonly exported to determine if these levels meet the current acceptable regulatory limits specified by each country. The health impacts from exposure to the four common metabolites B1, B2, G1, and G2 vary greatly based on the consumption level and exposure time with the aflatoxin metabolite, ongoing research goals are to identify if there is an impact on specific animal species or human age, sex, and health. An alternative methodology for sample cleanup is to bind the interfering compounds and immediately elute the aflatoxins from a non-gel, standard solid phase extraction (SPE) cartridge. The effectiveness of the Supel™ Tox AflaZea SPE Cartridges in combination with the SmartPrep Extractor System from Horizon Technology efficiently prepared a variety of foodstuffs samples representing a quadrant of moisture and viscosity levels prior to analysis using HPLC with fluorescence detection. Sample matrices chosen to represent the quandrant were almond milk, fresh corn, peanut paste, and curry powder were selected. Data presented concludes that aflatoxins B1, B2, G1, and G2 are effectively recovered using the novel and simple sample matrix preparation roadmap to meet both United States and European Union limits.
View here (1259568 KB)

A Novel Method for Pre-Column Derivatization of Aflatoxin B1, B2, G1, and G2 Prior to HPLC Analysis using the XcelVap® System as a Thermostatically-Controlled Heated Water Chamber
Aflatoxins, a mold largely produced by Aspergillus flavus and Aspergillus parasiticus1 are commonly tested mycotoxins found naturally in a wide range of agriculture crops and food products. Due to their harmful effects on human health, animal health, and global trade, aflatoxins are regulated in most countries and have established global limits in a wide variety of matrices2. Regulations for the maximum limits vary for the reported aflatoxin B1 and total aflatoxins (sum of B1, B2, G1, and G2); however, most countries importing food and agriculture products perform testing to approve the safety of products. Testing may often reveal aflatoxin levels above the maximum limits allowed, creating a trade restriction for certain agriculture and food products from certain countries3. The tests are performed according to their sampling methods and the results are measured against their established limits.There are several methods for detecting and quantifying aflatoxins; however, detecting all aflatoxins using the same method can be challenging. The limited response for B1 and G1 to naturally absorb UV light or fluoresce at the levels many countries need to quantify has created the need to add a derivatization step. To assist with detection at lower levels, derivatization of the aflatoxin standards using an acid solution aids in the fluorescence of both aflatoxin B1 and G1. Fluorescence is the more preferred reverse phase HPLC detection method for its ability to offer increased sensitivity at lower levels of aflatoxin.
View here (852565 KB)

You may search again if you were unhappy with your results. Just click the back button on your browser. Or click here.