LITERATURE


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LCMS-8050 Application - Analysis of Testosterone in Serum using LCMS-8050 (SSI)
Imtakt has optimized separation and detection characteristics utilizing the Shimadzu LCMS-8040 and LCMS-2020.
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Perfluorocarbons
The sensitivity of the LCMS-8030 was evaluated for ten perfluorocarbon compounds.
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LCMS-8030/8040 Application - Perfluorocarbons (SSI)
The sensitivity of the LCMS-8030 was evaluated for ten perfluorocarbon compounds.
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Quantitative Analysis of Cholesterol using LCMS-2020
Cholesterol was analyzed on the LCMS-2020 and a lower limit of quantitation (LLOQ) of 0.01 ppm was achieved.
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Fractionation by Preparative LC-MS and Fraction Verification byUltra Fast LC-MS
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Steroids: Testosterone, Progesterone, Estradiol, Ethinylestradiol
Sensitivity was tested for four steroids on the LCMS-8030 triple quadrupole mass spectrometer coupled with a Nexera UHPLC.
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LCMS-8040 Application - Pesticides in Cannabis
An LC-MS method for detection of pesticides in cannabis with QuEChERS extraction was developed.
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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.
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Analysis of Alprazolam, Reserpine and Verapamil Using the LCMS-8030 Triple Quad Mass Spectrometer
Analysis of Alprazolam, Reserpine and Verapamil Using the LCMS-8030 Triple Quad Mass Spectrometer
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Analysis of Carbohydrates with LCMS
LCMS with ESI ionization is a viable alternative for low-sensitivity analysis of carbohydrates of similar structure or molecular weight.Proper column and mobile phase selection produced peak resolution where needed as well as consistent ionization.
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LCMS-8050 Customer Applicaiton - Hepcidin Analysis on LCMS-8050 (SSI)
This shows an example of analyzing inorganic and hydrocarbons gases using a PLOT (porous layer open tubular) column.
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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.
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Analysis of a Peptide Mixture using the LCMS-8050 Triple Quadrupole Mass Spectrometer
A method for the rapid optimization and analysis of peptides was developed using an ultrafast LCMS-8050. Detection limits were in the low femtomolar range.
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LCMS-2020 Application - Quantitative Analysis of Cholesterol using LCMS-2020 (SSI)
This work demonstrates a rapid method for the detection and quantification of Cholesterol down to a LLOQ of 0.01ppm using a Shimadzu LCMS-2020.
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Quantitative Analysis of Glyphosate and AMPA using the LCMS - 8060
The Lower Limit of Quantitation for Glyphosate and its metabolite Aminomethylphosphonic Acid (AMPA) were tested on the LCMS-8060, reaching an LLOQ of 0.1 ppb without the need for derivatization.
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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.
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LCMS-8030/8040 Application - Quantitative Analysis of Cannabinoids using the LCMS-8040 Triple Quad MS (SSI)
A method for rapid quantitation of various cannabinoids was requested utilizing UHPLC equipment and LCMS to increase the speed and sensitivity of analysis.
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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
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Make sure you know what you're dealing with! - Analysis of phenoxypropionic herbicides using LCMS
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HPLC Techniques to Improve LCMS Performance and Productivity
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Quantitative Analysis of Carbohydrates by LC/MS
Here we introduce examples of quantitative analysis of carbohydrates in foods using post-column solvent addition.
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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.
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Designer Cannabinoids
A rapid LC-MS-MS method for determination of designer cannabinoids in smokeable herbs was developed.
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Mycotoxins
An extremely fast LC-MS-MS method for the determination of mycotoxins and other untargeted chemical threats was developed.
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Protein and Peptide Analysis
Amyloid Beta 1-40, Insulin, Salmon Calcitonin, and NPY1-36
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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.
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LCMS Sample Evaluation Report
This report demonstrates the chromatographic performance and LCMS analysis for components of customer-provided samples. Utilizing the LCMS-2020, the objective was to attain resolution of 5 components from test mix in a total method runtime of 2 minutes or less, including MS spectral peaks.
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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.
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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.
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LCMS-2020 Application - Analysis of Digoxin, Nadolol and Metoprolol Using a Fast Polarity Switching DUIS Method (SSI)
Qualification and quantitation of isobutrin and butein in rabbit plasma samples were tested using the LCMS-2020 single quadrupole mass spectrometer. A LCMS method was developed and analyzed for these two standards.
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LCMS-8030/8040 Application - Benzodiazepines and Barbiturates (SSI)
Qualitative analysis of three marker and nine unknown compounds in were tested using the LCMS 2020 single quadruple mass spectrometer using a dual ion source (DUIS). In addition, quantitation of the marker compound digoxin was also tested. An LCMS method was developed and analyzed for all compounds in these samples.
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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.
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LCMS-8040 Application - Simultaneous Analysis of Amino Acids and Acylcarnitines in DBS (Dried Blood Spot) with LCMS-8040 (Japan)
Here we describe an analysis performed using an LCMS-8040 high-performance liquid chromatograph-triple quadrupole mass spectrometer and employing an analytical protocol used by the Mass Spectrometry, Clinical Chemistry and Pharmacology Lab of Meyer Children’s Hospital.
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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.
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LCMS-8050 Application - Quantitative Analysis of Microcystin Cyclopeptides Using the Ultra-Fast Triple Quadrupole LCMS-8050 EPA 544 (SSI)
The following describes the use of a gas chromatograph (GC) equipped with a Phaser Olfactory GC Port that enables food companies to standardize food flavor and concentration.
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LCMS-8050 Application - Quantitative Analysis of Fluorotelemer Alcohols using the LCMS-8050 (SSI)
Quantitative analysis of an example fluorotelomer alcohol (FTOH) was conducted using the LCMS-8050 triple quadrupole mass spectrometer. A lower limit of quantitation (LLOQ) of 0.5ppb and a level of detection (LOD) of 0.1ppb was achieved for 7:2-sFTOH in neat solution.
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LCMS-8060 Application - A Rapid LCMS Method for Evaluation of EPA 1694 and 6810 Contaminants in Drinking Water (SSI)
An ultra-fast polarity switching #31;ve minute method to analyze and quantify many different contaminants of emerging concern (CECs) by LCMS-MS.
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LCMS-8060 Application - Shimadzu’s Guide to US DOD_DOE Analysis of PFCs using the LCMS-8060
Quantitative analysis of Perfluorinated Compounds (PFC’s) by US DOD/DOE QSM v5.1 with and without the use of solid phase extraction for sample preparation was conducted using the LCMS-8060 triple quadrupole mass spectrometer.
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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
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Analysis of Polymer Additives Using LCMS-2020
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.
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Structural analysis of 26 pharmaceutical compounds using synchronized survey scan measurement using the LCMS-8030 Triple Quad Mass Spectrometer
Structural Analysis of 26 Pharmaceutical Compounds using synchronized survey scan measurement.
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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
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LCMS-8030/8040 Application - Serotonin (Japan)
This bulletin introduces the following data, acquired with respect to standard anionic surfactant solutions, utilizing the Shimadzu Prominence HPLC / RF-20A fluorescence detector.
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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.
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Identification of Benzodiazepines and Their Metabolites Using Synchronized Survey Scan®
This report describes the analysis of benzodiazepines and their metabolites using ultra-high speed triple quadrupole mass spectrometry (LCMS-8030).
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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.
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Analysis of 90 Multi-Class Drugs with Polarity Switching in Plasma
Ninety drugs and internal standards were prepared in plasma using a Biotage SLE 96-well plate and analyzed on an LCMS-8050.
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Simultaneous Ultrafast Analys is for Research of Anti-Cancer Drugs
Three anti-cancer drugs were prepared in plasma using a Biotage® SLE 96-well plate and analyzed on an LCMS- 8050.
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Simultaneous Qualitative and Quantitative Data Acquisition for Research of Diabetes Drugs
By utilizing the LCMS-8050’s ultrafast scan speed, both quantitative and qualitative data were acquired for 5 drugs simultaneously without the need for an ion trap.
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Simultaneous Analysis of Irganox Polymer Additive using LC-MS
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Analysis of Phenoxyproprionic Type Herbicides using LC-MS
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Analysis of Bisphenol A Diglycidyl Ether Using LC-MS
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Analysis of Microcystins Using LC-MS
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Drug analysis using Co-Sense for BA LC-MS system (1)
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Analysis of fullerenes using LC-MS
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Analysis of alkyl phenyl polyoxyethylene sulfonate using LC-MS
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Analysis of benzalkonium and polyoxyethylene lauryl ether using LC-MS
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Analysis of fatty acid amidopropylbetaine using LC-MS
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Analysis of pesticides in foods using LC-MS
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Structure elucidation of trace amount of impurities in drugs using Co-Sense for LCMS system analogue
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Analysis of alkylphenols using LC-MS
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Analysis of Vitamin K in food using LC-MS
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Analysis of penicillin analogue using LC-MS
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Analysis of Bisphenol A and Nonylphenol using LC-MS
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Analysis of DNPH-aldehydes using LC-MS
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Analysis of antioxidants in drug and food using LC-MS
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Analysis of Proteins and Peptides using LC-MS
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Analysis of Sudan Dyes and Para Red using LC-MS
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Accurate Mass Analysis of Flavonoids by LCMS-IT-TOF
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Analysis of Steroidal Anti-Inflammatory Drugs Using LC/MS
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Drug Analysis Using “Co-Sense for BA” LC/MS System (2)
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Simultaneous Analysis of Pesticides in Environment Water using LC-MS
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Simultaneous Analysis of Pesticides using LC-MS
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Analysis of Catechins Using LCMS-2010EV
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Simultaneous Detection by MS, PDA and Fluorescence Detectors with LCMS-2010A System
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Simultaneous Analysis of Carbamate Pesticides with LC-MS
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Analysis of N-nitroso-fenfluramine using LC-MS
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Analysis of aflatoxins using LCMS-2010A
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Screening for bioactives compounds by means of ESI-MS
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Application using Analytical / Preparative LC-MS System (Part 1)
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Analysis of Perfluorochemicals (PFOA, PFOS) using LC-MS
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Accute poisoning with a rat bait
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Which column is your analysis based on?
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Natural Product Analysis using the LCMS-IT-TOF
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Opening LCMS to research: Psiport browser software
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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.
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[ARCHIVED] LCMS Sample Evaluation Report - Roark Galloway & Miguel Gallego (SSI)
Two samples were submitted to the Shimadzu Southern California (SCA) regional laboratory to demonstrate chromatographic performance and LCMS analysis for components of those samples. The samples were prepared and provided by representatives from CONFIDENTIAL Research Laboratories for this evaluation. The samples were identified as: 1) Test mix (5 components) 2) Sample ID- A001
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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.
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Analysis of Water-Soluble Vitamins with Multi-Mode ODS Column Using LCMS-2020
Here we present an example of analysis of 8 watersoluble vitamins using a cation exchange-anion exchange multi-mode ODS column, (Scherzo SM-C18, Imtakt Corporation) in conjunction with the LCMS2020 mass spectrometric detector. The gradient consisted of formic acid / ammonium formate buffer and acetonitrile mobile phases, components typical for high sensitivity reverse-phase LCMS analysis.
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Analysis of water soluble water vitamins using the LCMS-8030 Triple Quad Mass Spectrometer
Analysis of Water Soluble Water Vitamins using the LCMS-8030 Triple Quad Mass Spectrometer. Vitamins include Thiamin, Pyridoxin, Riboflavin, Folic Acid and many more.
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Analysis of fat soluble vitamins using the LCMS-8030 Triple Quad Mass Spectrometer
Analysis of fat soluble vitamins using the LCMS-8030 Triple Quad Mass Spectrometer. Vitamins include: Vitamin A, Vitamin D2, Vitamin D3, Vitamin K1 and many more.
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Fast precursor ion scan and neutral loss measurement of sulfa drugs using the LCMS-8030 Triple Quad Mass Spectrometer
Fast Precursor Ion Scan and Neutral Loss Measurement of Sulfa Drugs Using the LCMS-8030 Triple Quad Mass Spectrometer.
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LCMS-2020 Application - Analysis of Chloramphenicol in Honey Using LCMS-2020 (Japan)
In this issue, we describe the light source, an important part of the spectrophotometer that was explained in “The Structure of a Spectrophotometer” in UV Talk Letter Vol 2”
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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.
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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.
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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.
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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.
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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.
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LCMS-IT-TOF Application - Electroplating Bath Analysis (SSI)
Using the Shimadzu LCMS-8030 triple quadrupole mass spectrometer, efficient and accurate methods have been developed to identify and quantify trace amounts of 13 pesticides found in fruits and vegetables.
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Analysis of Human IgG using Automated Digestion Coupled Directly to LCMS-8050
Quantification of human IgG using an automated online trypsin digestion platform coupled directly to LCMS-8050 triple quadrupole mass spectrometer was performed. Two common peptides for IgG were monitored and the limits of detection were in the low fmol levels on column.
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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.
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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.
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LCMS-8050 and LCMS-IT-TOF Application - Online Affinity and Digestion: A Flexible and Robust Tool for the Characterization and Quantification of Proteins (SSI)
Rapid collection and screening methods for the pain management market are necessary due to the high throughput nature and rapid result requirements. Measuring these compounds in oral fluid has typically been shown to be more difficult but preferable to analyzing these compounds in urine.
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LCMS-8050 Application - Vitamin D3 and Related Compounds by ESI and APCI (SSI)
Quantitative analysis of vitamin D2 and vitamin D3 was conducted using the LCMS-8040 triple quadrupole mass spectrometer. A lower limit of detection (LLOD) of 10pg on column was achieved for both compounds.
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LCMS-8050 Application - Quantitative Analysis of Pyrethroids in Soil and Sediment Using the Shimadzu LCMS-8050 Triple Quadrupole Mass Spectrometer (Japan)
Here, simultaneous analysis of these four pesticides in a standard sample was conducted in compliance with the Separate Method 9 using Prominence-I integrated high-performance liquid chromatograph, and the measurement accuracy and linearity were then evaluated.
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Quantitative Analysis of Natural Cannabinoids using the Triple Quad LCMS-8050
Quantitative analysis of natural cannabinoids was conducted using the LCMS-8050 triple quadrupole mass spectrometer. A lower limit of quantitation (LLOQ) of 1 – 4 ng/mL was achieved depending on the specific cannabinoid. This method showed certain medicinal oils or tinctures available over the internet contained naturally occurring cannabinoids.
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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.
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LCMS-8060 Application - Analysis of Nitrosamines Using LCMS-8060 Triple Quadrupole Mass Spectrometer
Hexanoate ester derivatized 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL) and its D3 labeled internal standard are quantitatively measured out of a urine matrix using the LCMS-8060.
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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.
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LCMS-8060 Application - Quantitative Analysis of Glyphosate and AMPA using the LCMS - 8060 (SSI)
The Lower Limit of Quantitation for Glyphosate and its metabolite Aminomethylphosphonic Acid (AMPA) were tested on the LCMS-8060, reaching an LLOQ of 0.1 ppb without the need for derivatization.
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Analysis of Nitrosamines using LCMS-8060 Triple Quadrupole Mass Spectrometer
Hexanoate ester derivatized 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL) and its D3 labeled internal standard are quantitatively measured out of a urine matrix using the LCMS-8060.
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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.
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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.
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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.
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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.
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Qualitative Analyses of Pharmaceuticals Utilizing a New
An important instrument capability for qualitative analysis is a collision-induced disassociation (CID). CID is achieved on the Shimadzu LCMS QP-8000 by increasing the kinetic energy of the ion beam in order to fragment intact quasi-molecular and adduct ions on the skimmer.
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Analysis of Impurities of Ru Dye (N719) for Dye-Sensitized Solar Cells
Here we introduce an example of the separation and qualitative analysis of impurities in the widely used dye, Ru N719, using the LCMS-2020.
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Electroplating Bath Analysis
The formula of substances in an unknown mixture were predicted using an ion trap time-of-flight mass spectrometer with accurate mass and accurate MSn capability.
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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.
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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.
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LCMS-8030/8040 Application - Mycotoxins (SSI)
A rapid LC-MS-MS method for determination of designer cannabinoids in smokeable herbs was developed.
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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.
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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)
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Accelerating quantitative proteomics analysis with Shimadzu UFMS and Skyline
The Key challenge for quantitative proteomics researchers is to accurately quantitate proteins and peptides in complex biological systems with high sensitivity. Multiple reaction monitoring (MRM) is the main current approach for highly confident protein and peptide quantification.
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Analysis of a drug in plasma using ON-LINE pretreatment method to remove proteins for LC-MS
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Bisphenol A-consumption inevitable - Fast determination of bisphenol A residues in plastic bottles, containers and cans
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A good connection - Integrated in an online system: sample preparation and HPLC-MS analysis of biological samples
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Organ transplantation - Determination of sirolimus and tacrolimus with HPLC/MS in whole blood
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Simultaneous determination of tryptophan, phenol, p-cresol and cholic acid in pretreated human blood
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Identification of unknown polymer additives using LCMS-IT-TOF
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Analytical Instrument Validation According to Food Safety Management System (ISO 22000)
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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.
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LCMS-2020 Application - Analysis of Polymer Additives Using LCMS-2020 (Japan)
Here we present an example of analysis of 8 watersoluble vitamins using a cation exchange-anion exchange multi-mode ODS column, (Scherzo SM-C18, Imtakt Corporation) in conjunction with the LCMS2020 mass spectrometric detector. The gradient consisted of formic acid / ammonium formate buffer and acetonitrile mobile phases, components typical for high sensitivity reverse-phase LCMS analysis.
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LCMS-2020 Application - Analysis of Water-Soluble Vitamins with Multi-Mode ODS Column Using LCMS-2020 (Japan)
Here we present an example of analysis of 8 watersoluble vitamins using a cation exchange-anion exchange multi-mode ODS column, (Scherzo SM-C18, Imtakt Corporation) in conjunction with the LCMS2020 mass spectrometric detector. The gradient consisted of formic acid / ammonium formate buffer and acetonitrile mobile phases, components typical for high sensitivity reverse-phase LCMS analysis.
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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.
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LCMS-8050 Application - Rapid and Reproducible Analysis of Peptides using the Triple Quad LCMS-8050 (SSI)
Quantitative analysis of natural cannabinoids was conducted using the LCMS-8050 triple quadrupole mass spectrometer. A lower limit of quantitation (LLOQ) of 1 – 4 ng/mL was achieved depending on the specific cannabinoid. This method showed certain medicinal oils or tinctures available over the internet contained naturally occurring cannabinoids.
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LCMS-8050 Application - Analysis of a peptide mixture using the LCMS-8050 (SSI)
Quantitative peptide analysis of in protein mixtures is becoming a routine tool for the analysis of biological samples. In order to quantitatively analyze peptide products in a complex mixture, a method incorporating fast dwell and pause times is required, as is the ability to concurrently measure a number of targets including stable isotope labeled peptide internal standards. This application describes the use of the LCMS-8050 in conjunction with Skyline and LabSolutions to carry out rapid method optimization and detection of commercial peptide standards in a mixture.
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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.
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LCMS-8030/8040 Application - Simultaneous Measurement of Positive-Negative Ions of 30 Pesticides for Water Management Using the LCMS-8030 Triple Quadrupole Mass Spectrometer (Japan)
Here we investigated RNA sequencing analysis using the acid-hydrolysis method.
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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.
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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.
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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.
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LCMS-2020 Application - Analysis of Impurities of Ru Dye (N719) for Dye-Sensitized Solar Cells( Japan)
Here we introduce examples of impurity analysis of nitrendipine and nifedipine using the Prominence UFLC and LCMS-2020.
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Screening of plastic additives using the LCMS-8030 Triple Quad Mass Spectrometer
This note describes full scan analysis of a mixture of 12 plastic additives using Synchronized Survey Scan (SSS) as shown in Figure 1. High-speed polarity Switching (15 msec) and rapid scan rates (10000 u/sec) allow multiple collision energies to be employed for automatic product ion scanning .
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Screening of sulfa drugs using the LCMS-8030 Triple Quad Mass Spectrometer
This document describes a method of screening for sulfa drugs using precursor (hereinafter called Prec.) and neutral loss (hereinafter called NL) scans.
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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.
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LCMS-8030/8040 Application - Quantitative analysis of hydrophilic metabolite using ion-paring chromatography with a high-speed triple quadrupole mass spectrometer (Japan)
Here, we present the analysis method of degradation products generated in electrolyte using high mass accuracy MSn and multivariate statistical technique.
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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.
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LCMS-2020 Application - A Fast Dual Ion Source (DUIS) Method for Analysis of Isobutrin and Butein in Rabbit Plasma Samples (SSI)
Here we report the results of analysis of a mixture of organic acids using a dual-column, dual-temperature method.
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LCMS-8040 Application - Development of a Comprehensive Detection Method of Eicosanoids and Platelet Activating Factor Using Ultra-High Performance Liquid Chromatography/Mass Spectrometry (Japan)
Using LCMS-8040, simultaneous detection method of eicosanoids and PAF was developed. 54 MRM transitions for 50 eicosanoids and PAF (platelet activation factor) were optimized. Limit of quantitation for several targets was in the subpicogram range.
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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.
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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.
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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.
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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.
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LCMS-8030 Application - Identification of Drugs in Urine Using Synchronized Survey Scan (Japan)
This report describes the analysis of benzodiazepines and their metabolites using ultra-high speed triple quadrupole mass spectrometry (LCMS-8030).
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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.
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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.
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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”.
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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
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LCMS-8050 Application - High-Speed Analysis of Sunitinib and Axitinib in Plasma Using Triple Quadrupole LCMSMS (LCMS-8050) (Japan)
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 pretreatment was used that involves only deproteinizaiton, the quantitative results obtained were excellent in terms of accuracy and precision.
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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.
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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.
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LCMS-8050 Applicaiton - Analysis of Human IgG using Automated Digestion Coupled Directly to LCMS-8050 (SSI)
This report examines the repeatability and linearity of a standard ethanol solution, and confirms the separation of other oxygenated compound standard solutions. The analysis presented here was performed using the HS-20 and the Rtx-BACPlus series of high-separation columns specifically designed for the analysis of alcohol in blood.
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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.
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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.
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LCMS-8050 Application - Pain management panel in oral fluids using the LCMS-8050 with polarity switching (SSI)
Rapid collection and screening of THC has quickly become necessary because of the nationwide push for the legalization of Marijuana. Many oral fluid methods struggle to meet the demands of the customer due varying factors, some of which include sensitivity, speed of analysis, or cost. In states where Marijuana is legal, law enforcement agencies have a great need for a fast, sensitivity, and cost effective method in order effectively enforce laws such as D.U.I.D. where evidence preservation is absolutely critical.
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LCMS-8030/8040 Application - Analysis of Carboxy THC Using the LCMS-8030 Triple Quadrupole Mass Spectrometer (SSI)
MALDI TOF analysis is rapidly gaining attention in the field of molecular imaging and microbiology. Tissue sections, whole microorganisms and other biological material are now routinely being deposited onto MALDI plate, coated with a matrix compound and inserted directly into the MALDI TOF instrument. From an analysis perspective these biological materials are very ‘dirty’ samples compared for example to more traditional MALDI TOF samples such as protein digests or peptides.
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LCMS-2020 Application - Quantitative Analysis of Cannabinoids using the LCMS-2020 Single Quad MS (SSI)
Brominated flame retardants are widely used and contained in electric and electronic devices, and are to be controlled under the Restriction of Hazardous Substances (RoHS directive). If the quantitative analysis of them is done by thermal desorption-GC technique (TD-GC), a various measurement parameters need to be optimized. In this report, the temperature optimization for Py-GC interface (ITF) and GC injection port is described.
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LCMS-8040 Application - Quantitative Analysis of Vitamin D2 and D3 using the LCMS-8040 (SSI)
By using the Nexera-e with a photodiode detector (PDA), a target component can be separated from a complicated mixture of coexisting substances, and then quantitated, all in a single analysis. In the analysis, assuming ethyl gallate, tyrosol and rutin as the target compounds, the ChromSquare dedicated software was applied to generate a contour plot using the respective optimal wavelengths, thereby permitting both separation and quantitation.
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LCMS-8050 Application - Quantitative Analysis of Natural Cannabinoids using the Triple Quad LCMS-8050 (SSI)
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
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LCMS-8050 Application - Comprehensive Monitoring Method for Analyzing 158 Lipid Mediator Species Using the Ultra-Fast LCMS-8050 (Japan)
Accurate and sensitive characterization and quantification of a structurally diverse class of microcystin cyclopeptides was accomplished using UHPLC-MS-MS. In this analysis microcystins-RR, YR, and LR were measured using a Nexera UHPLC with a LCMS-8050 triple quadrupole MS detector with ESI ionization.
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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.
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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
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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.
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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.
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Analysis Using Dual Ion Source DUIS-2010 (Part 2)
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Analysis Using Dual Ion Source DUIS-2010(Part1)
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LC-MSAnalysis of Compounds Related to Nucleic Acids
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Analysis of Aminoglycoside Antibiotics(Gentamicins & Neomycin)(1)
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Analysis of Microcystins using LS-MS (No. 2)
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Ultra Fast Analysis (Part 2)Analysis of Impurities in Curcumin
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Structural Prediction of Impurities in Drugs using MSn Data
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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.
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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.
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Determination of a ß-Amyloid Protein Fragment
Mutation of the transthyretin, apolipoprotein or gelsolin plasma proteins results in various forms of familial amyloidsis polyneuropathy (FAP) by the build-up of anyloid fibrils of these associated proteins and protein precursors in the human nervous system and other tissues.
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ESI Mass Spectra of Heme Proteins
The structure and function of the globular proteins including myoglobin and hemoglobin enable them to perform their functions of oxygen storage and transport and are thought to be evolved from a common ancestral oxygen-binding heme protien
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Colourful, but hazardous: forbidden dyes - Fast C/MS determination of Sudan Red I-IV, butter yellow and Para Red in foods
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An apple per day keeps the doctor away - Mycotoxins are a world-wide problem - Highly sensitive determination of the fungal toxin patulin
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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
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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.
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Structural Analysis of Glycopeptides (RNase B) Utilizing Accurate MSn Measurement
Glycoproteins are an essential component of cell membranes, and elucidation of their functions in relation to oncogenesis and/or viral infections is receiving attention in the search for cures, treatments, and vaccines. As glycoprotein diversity plays a key role in intercellular recognition, determination of sugar chain structure, and the sequence of amino acids bonded to sugar chains, is required for functional prediction. The LCMS-IT-TOF is ideal for sugar chain analysis as it is capable of producing high mass accuracy MSn spectra; this ability provides the power to elucidate the often complex sequences of these compounds. Moreover, analysis of small quantities of a biological sample is possible when combining the LCMS-IT-TOF with a nanoESI interface.
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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).
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LCMS-8030/8040 Application - Analysis of Water Soluble Vitamins Using the LCMS-8030 Triple Quadrupole Mass Spectrometer (Japan)
Ultra Fast Speed: Fusion of Ultra Fast MRM and Ultra Fast Polarity Switching An Ultra Fast Scan Speed of 15,000 u/sec 500 MRMs per Second, the Most Ever Possible. High Reliability: Robust System Provides Long-term Data Stability UFsweeperTM Technology Dramatically Minimizes Cross Talk Excellent Linearity with Wide Dynamic Range. User-Friendly: Easy Maintenance for Minimized Instrument Downtime Single-vendor Solution Provides Seamless Operation Quantitation Browser for Effective Multi-analyte Quantitation.
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LCMS-8030/8040 Application - Analysis of Alprazolam, Reserpine and Verapamil Usinf the LCMS-8030 Triple Quadrupole Mass Spectrometer (Japan)
Ultra Fast Speed: Fusion of Ultra Fast MRM and Ultra Fast Polarity Switching An Ultra Fast Scan Speed of 15,000 u/sec 500 MRMs per Second, the Most Ever Possible. High Reliability: Robust System Provides Long-term Data Stability UFsweeperTM Technology Dramatically Minimizes Cross Talk Excellent Linearity with Wide Dynamic Range. User-Friendly: Easy Maintenance for Minimized Instrument Downtime Single-vendor Solution Provides Seamless Operation Quantitation Browser for Effective Multi-analyte Quantitation.
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LCMS-8030/8040 Application - Analysis of Fat Soluble Vitamins Using the LCMS-8030 Triple Quadrupole Mass Spectrometer (Japan)
Ultra Fast Speed: Fusion of Ultra Fast MRM and Ultra Fast Polarity Switching An Ultra Fast Scan Speed of 15,000 u/sec 500 MRMs per Second, the Most Ever Possible. High Reliability: Robust System Provides Long-term Data Stability UFsweeperTM Technology Dramatically Minimizes Cross Talk Excellent Linearity with Wide Dynamic Range. User-Friendly: Easy Maintenance for Minimized Instrument Downtime Single-vendor Solution Provides Seamless Operation Quantitation Browser for Effective Multi-analyte Quantitation.
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LCMS-8030/8040 Application - Screening of Plastic Additives Using the LCMS-8030 Triple Quadrupole Mass Spectrometer (Japan)
Ultra Fast Speed: Fusion of Ultra Fast MRM and Ultra Fast Polarity Switching An Ultra Fast Scan Speed of 15,000 u/sec 500 MRMs per Second, the Most Ever Possible. High Reliability: Robust System Provides Long-term Data Stability UFsweeperTM Technology Dramatically Minimizes Cross Talk Excellent Linearity with Wide Dynamic Range. User-Friendly: Easy Maintenance for Minimized Instrument Downtime Single-vendor Solution Provides Seamless Operation Quantitation Browser for Effective Multi-analyte Quantitation.
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LCMS-8030/8040 Application - Fast Precusor Ion Scan and Neutral Loss Measurement of Sulfa Drugs Using the LCMS-8030 Triple Quadrupole Mass Spectrometer (Japan)
Ultra Fast Speed: Fusion of Ultra Fast MRM and Ultra Fast Polarity Switching An Ultra Fast Scan Speed of 15,000 u/sec 500 MRMs per Second, the Most Ever Possible. High Reliability: Robust System Provides Long-term Data Stability UFsweeperTM Technology Dramatically Minimizes Cross Talk Excellent Linearity with Wide Dynamic Range. User-Friendly: Easy Maintenance for Minimized Instrument Downtime Single-vendor Solution Provides Seamless Operation Quantitation Browser for Effective Multi-analyte Quantitation.
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LCMS-8050 Application - Vitamin D3 Data Presentation for LCMS-8050 (Asia Pacific)
Aldehydes and ketones in the environment can be analyzed using HPLC by derivatizing them with 2,4-dinitrophenylhydrazine (2,4-DNPH). For multicomponent separation of aldehyde/ketone DNPH derivatives, reverse‐phase gradient elution is generally used. 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 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).
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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.
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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.
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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.
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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.
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LCMS-8030 Application - Screening and Individual Quantitative Works of Regulated Substances in Food Using Triple Quadrupole Mass Spectrometer LCMS-8030 (Japan)
In this Technical Report, we used the LCMS-8030 triple quadrupole mass spectrometer to evaluate whether or not 10 pesticide compounds used to spike a matrix at 10 ppb each could be detected automatically by using generic peak detection method in the screening for 176 pesticides using 1 msec pause and 5 msec dwell times.
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LCMS-IT-TOF Application - Determination of Industrial Dyes in Food by LCMS-IT-TOF (China)
Structure elucidation using tandem mass spectrometry is dominated by approaches that use accurate mass, parent-ion isolation and fragmentation or a combination of both. MS3 is useful as it allows intermediates in fragmentation pathways to be the assigned but is limited for real-time analysis by lack of speed and consequent loss of peak definition and quantitative reproducibility, particularly for UHPLC. We have applied UFMS2 to generate multiple spectra for on-the-fly detection and identification of pharmaceutical compounds and metabolites.
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LCMS-8040 Application - Measurement of Fumaryacetaoacetate Activity in DBS (Dried Blood Spot) with LCMS-8040 (Japan)
In this study, we report a developed analytical system using ultra-high speed triple quadrupole mass spectrometry with a new extraction method for pretreatment in forensic analysis. The system has a sample preparation utilizing modified QuEChERS extraction combined with a short chromatography column that results in a rapid run time making it suitable for routine use.
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LCMS-8040 Application - Measurement of Methylmalonic Acid, 3-OH Propionic Acid and Succinic Acid in DBS (Dried Blood Shot) with LCMS-8040 (Japan)
Here we describe an example analysis for succinylacetone performed using an LCMS-8040 high-performance liquid chromatograph-triple quadrupole mass spectrometer and employing an analytical protocol used by the Mass Spectrometry, Clinical Chemistry and Pharmacology Lab of Meyer Children’s Hospital.
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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.
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LCMS-8040 Application - Analysis of D- and L-amino acids using Automated Pre-Column Derivatization and Liquid Chromatography-Electrospray Ionization Mass Spectrometry (Japan)
This report describes an analytical system using ultra-high-speed triple quadrupole mass spectrometry (LCMS- 8030) for forensic analysis of drugs in urine. The LCMS-8030 has a Synchronized Survey Scan function that automatically performs MS/MS when a precursor threshold is exceeded, thereby producing a combined MRM and MRM-dependent product ion scan in a single analysis.
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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.
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LCMS-8030 Application - Identification of Benzodiazepines and Their Metabolites using Synchronized Survey Scan (Japan)
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.
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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.
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LCMS-8050 Application - High Sensitivity Detection and Polarity Switching of 50 pg of Trenbolone and Ethynyl Estradiole using the LCMS-8050 (SSI)
Recent innovations with Skyline have resulted in a version of Skyline that can upload and analyze *.lcd files directly. We applied this analysis to demonstrate the integration of Shimadzu products into the Skyline environment. Using this workflow, we identified CVs of less than 2 % for several experimental approaches.
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LCMS-8050 Application - Analysis of Steroids and NSAIDs Using the Shimadzu LCMS-8050 Triple Quadrupole Mass Spectrometer (Japan)
Foods in which chemical residues, like pesticides, feed additives, and veterinary drugs found in excess of maximum residue levels have been banned from sale in many countries around the world. Compounds that are subject to residue standards vary widely and the list is expected to grow. Because of this, there is a need for a highly sensitive and rapid analytical technique to analyze as many of these compounds as possible in a single run. This application News introduces an example of the high-sensitivity analysis of 89 veterinary drugs in a crude extract of livestock and fishery products.
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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).
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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.
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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.
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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.
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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.
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LCMS-8050 Application - Simultaneous Qualitative and Quantitative Data Acquisition for Research of Diabetes Drugs (SSI)
Diabetes has an impact on the lives of a large number of people worldwide and thus has generated a need for high quality data for research. As the need for more data coincides with ever increasing laboratory costs, the ability to efficiently extract data has become more important than ever. The speed of the LCMS-8050 allows for quantitative data to be acquired while also simultaneously acquiring qualitative scans that can be used for further confirmation or to further research. Here we acquire product ion scans during MRM acquisition to add an additional layer of confirmation. This can then be compared to a library search or visual examination.
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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.
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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.
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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.
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LCMS-8050 Application - Analysis of Cartap, Pyracolonil, Ferimzone in Drinking Water Using the Triple Quadrupole LCMS-8050 (Japan)
This article describes an example of inspecting samples for these three components by simultaneous analysis using a liquid chromatograph-mass spectrometer system, as specified in Appendix Method 20-2. Cartap decomposes to nereistoxin. Ferimzone includes type E and Z isomers, the concentrations of which are totaled to determine the Ferimzone concentration.
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Quantitative Analysis of Microcystin Cyclopeptides Using the Ultra-Fast Triple Quadrupole LCMS-8050- EPA Method 544
Accurate and sensitive characterization and quantification of a structurally diverse class of microcystin cyclopeptides was accomplished using UHPLC-MS-MS. In this analysis microcystins-RR, YR, and LR were measured using a Nexera UHPLC with a LCMS-8050 triple quadrupole MS detector with ESI ionization in accordance with EPA Method 544. Analysts should refer to EPA 544 for sample collection, preservation, holding time, extraction, and quality control measures.
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LCMS-8050 Application - Simultaneous Assay of Multiple Synthetic Contraceptive Hormones in Human Serum by LCMS-MS (SSI)
Immunoassay is the conventional method for measuring steroid hormone levels in the clinical laboratory. Recently, the questionable sensitivity of some immunoassays and the desire for more sensitive methods has led to the need to develop alternative methods for measuring steroid hormones in human serum samples. In some cases, as with synthetic steroid hormones used for female contraceptive hormones, there are no reliable immunoassays available. This poster describes a comprehensive method for evaluating multiple synthetic steroids in serum using ultra-high performance liquid chromatography-tandem mass spectrometry (LCMS-MS).
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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.
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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.
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Metabolite Profiling of Arabidopsis by Shimadzu LCMS-IT-TOF with Phenomenome Profiler software
Biological function is the sum of gene interactions and metabolic network interactions; both are affected by the environment and genetics. Metabolomics can detect cryptic changes and link unpredictable phenotypes to their biochemistry. With the Shimadzu LCMS-IT-TOF, we can acquire high resolution and high mass accuracy in the MS data to help identify novel metabolite discovery.
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Structural Analysis of Reserpine Degradation Products by LCMS-IT-TOF
Structural elucidation of impurities during the development of pharmaceutical products is very important. While NMR and other techniques can be used for this purpose, the mass spectrometer is the primary means of conducting structural analysis. In order to do this, high mass accuracy with MSn fragmentation data is absolutely necessary.
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Accurate Mass Measurement of High Concentration Samples by LCMS-IT-TOF
This investigation shows that ASC function is an effective tool for preventing loss of mass accuracy due to saturation of the detector. Using ASC, highly accurate measurement results can be obtained in a single analysis in cases where the concentration is unknown or when the sample contains a mixture of components at varying concentrations.
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LCMS-2020 Application - Ultra High Performance Liquid Chromatography / Mass Spectrometry Using Open Solution Software (Japan)
Here we introduce an evaluation of ion detection sensitivity in analysis of an actual sample consisting of an O-linked glycopeptides, in addition to analysis of the glycosylation site.
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LCMS-2020 Application - Dual Ion Source DUIS-2020 for Simultaneous ESI and APCI Measurments (Japan)
Here we introduce an example of mass spectrometric analysis of a sample consisting of selectively collected protein C-termini, demonstrating a newly developed, successful method of amino acid sequencing.
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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.
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LCMS-2020 Application - Impurity Analysis of Drugs Using Shim-pack XR-Phenyl Column (Japan)
This document describes a method of screening for sulfa drugs using precursor (hereinafter called Prec.) and neutral loss (hereinafter called NL) scans.
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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.
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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.
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Impurity Analysis of Drugs Using Shim-pack XR-Phenyl Column
Selection of the appropriate column and setting the separation conditions are extremely important in impurity analysis. Although an ODS column is used most of the time, use of phenyl columns is increasing recently with the aim of improving separation. In particular, it is believed that the effectiveness of many pharmaceutical substances is linked to utilization of the aromatic ring π-π interaction. Here we introduce examples of impurity analysis of nitrendipine and nifedipine using the Prominence UFLC and LCMS- 2020.
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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.
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LCMS-8030/8040 Application - Setting Optimum Dwell, Pause, and Scan Event Times on the Shimadzu-8030 (SSI)
Amino acids contained in a sports drink were treated with EZ:faastTM (Phenomenex, Inc.), which enables easy pretreatment, and then analyzed by GC-MS.
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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.
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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.
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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.
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LCMS-8030/8040 Application - Rapid UHPLC-MS/MS Method for Characterization and Quantification of Quorum Sensing Signalling Molecules in Complex Environmental Samples (Asia Pacific)
The present study evaluated the metabolic profile of troglitazone and endogenous metabolites in the PXB compared to control mice (severe combined immunodeficiency - SCID) using high mass accuracy MS/MS analysis.
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LCMS-8030/8040 Application - Analytical method and MRM database development using online SPE-LCMSMS for screening anti-cancer drugs and metabolites in hospital's wastewatrers and rivers (France)
Here, a UHPLC-MS/MS method is developed to overcome the limitations of the biosensor-based AHL detection.
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LCMS-IT-TOF Application - Identification of novel pyrimidine ring cleavage metabolites of Buspirone via Spectral Similarity correlation score (UK)
In this Application Datasheet, an analysis of metabolites in rat urine is performed using GC-MS/MS. Results comparing this data with GC-MS data are also introduced.
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LCMS-IT-TOF Application - Analysis of trace amount of 17-B-Estradiol and its metabolites in aqueous samples using online-SPE and accurate MSn analysis (Japan)
This poster will discuss the use of an automated sample preparation system coupled to mass spectrometry to quickly and reproducibly identify differences between normal and abnormal hemoglobin.
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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.
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LCMS-IT-TOF Applicaiton - Analysis of degradation products in electrolyte for rechargeable lithium-ion battery through high mass accuracy MSn and multivariate statistical technique (Japan)
In this study we have developed a qualitative analytical system with online solid phase extraction (online-SPE) and accurate MSn analysis.
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LCMS-IT-TOF Application - Differential Analysis in vulcanizing accelerators for rubber products by high mass accuracy MSn and multivariate statistical technique (Japan)
In this study we report a new high resolution separating method for the simultaneous analysis of etizolam, triazolam and their metabolites.
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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.
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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.
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LCMS-8030 Application - Rapid and Highly Sensitive Quantitative Analysis and Screening of Aflatoxins in Foods Using Liquid Chromatography Triple Quadrupole Mass Spectrometry (Japan)
In this paper we have applied a 1 mm inside diameter column phase to the analysis of linear alkylbenzene sulfonate anion surfactants using a high speed MS/MS detection system.
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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.
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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.
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LCMS-8030 Application - Screening of Pesticides in Water Using SPE On Line (Italy)
Here, we report a new GC-MS/MS method using Multiple Reaction Monitoring (MRM) mode for simultaneous detection and quantification of six N-nitrosamines including NDMA for enhanced selectivity and sensitivity from the potential matrix interferences in beer samples.
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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.
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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.
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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.
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Perfinity and LCMS-IT-TOF Application - Overcoming Challenges of Protein Sample Preparation for Food Allergen Analysis (SSI)
This study of 8 water soluble vitamins seeks to determine the stability of a vitamin extract over a 12 hour period.
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LCMS-8040 Application - Rapid, High Throughput Quantitation of Thujone in Absinthe by UHPLC-MS-MS (SSI)
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 using o-phthalaldehyde (OPA). Here, we introduce an example of the analysis of fluorescent amines that were derivatized with OPA.
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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.
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LCMS-8040 Application - Determination of d9-Tetrahydrocannabinol and Two of its Metabolites in Whole Blood, Plasma and Urine by UHPLC-MS/MS using QuEChERS Sample Preparation (France)
We have developed analytical method for four immunosuppressants (Tacrolimus, Rapamycin, Everolimus and Cyclosporin A) with two internal standards (Ascomycin and Cyclosporin D) using ultra-fast mass spectrometer.
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LCMS-8050 Application - Fast and Highly Sensitive Analysis of Multiple Drugs in Ground-, Surface- and Wastewater (Germany)
Here we report a simple and reliable method for quantitation and characterization of polysorbate 80 in biotherapeutic products using two-dimensional HPLC.
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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.
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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.
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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.
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LCMS-2020 Application - Applications of Desportion Corona Beam Ionization Mass Spectrometry (China)
In this study, we tested three kind of samples: baby milk powder, milk thickening cereals ( our, rice and tapioca) and a vegetable puree mixed with cereals
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LCMS-IT-TOF Application - Characterization of Metabolites in Microsomal Metabolism of Aconitine by High Performance Liquid Chromatography/Quadrupole Ion Trap/Time of Flight Mass Spectrometry (China)
Systematic optimization of unique variables effect of a new triple quadrupole mass spectrometer for protein multiple reaction monitoring (MRM).
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LCMS-IT-TOF Application - Identification of Intermediates from Ozone Oxidation of Oseltamivar Phosphate using an Ion-Trap Time of Flight Mass Spectrometer (Korea)
The aim of our work was to obtain the metabolic pathways of AC by the human liver microsomes.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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LCMS-8050 Application - Application of a sensitive liquid chromatography-tandem mass spectrometric method to determination of octreotide in human plasma (China)
A fast and sensitive method for octreotide in human plasma by ultra high performance liquid chromatography-tandem mass spectrometry was developed. The lower limit of quantitation was 5.0 pg/mL and the results of other parameters for method validation were good.
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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.
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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.
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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.
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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.
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LCMS-8050 Application - Metabolomic Approach for Carotenoids Analysis of Chrysanthemum flow by LCMS
Here we demonstrate the metabolomic analysis for carotenoids in Chrysanthemum flower as a model samples by a liquid chromatograph tandem mass spectrometry. Under this situation, a metabolomic approach of carotenoids was investigated to establish the metbolomic platform using liquid chromatograph tandem mass spectrometry in order to develop novel and efficient breeding process for horticulture plant.
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Analysis of Amoxicillin using the LCMS-2010EV and the LCMS-IT-TOF
<p>Amoxicillin is a drug belonging to a class of compounds known as b-lactam antibiotics.&nbsp; Amoxicillin, a member of the penicillin family, is used most often to treat a number of bacterial infections including H. influenzae, N. gonorrhoea, E. coli, Pneumococci, Streptococci, and some strains of Staphylococci.&nbsp; It is thought that these penicillin-derived compounds work to stop the bacteria from multiplying by inhibiting its cell wall synthesis.&nbsp; </p>
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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.
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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.
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LCMS-8050 Application - Analysis of 113 Multi-Class Drugs with Polarity Switching on LCMS-8050 (SSI)
Currently, the analytical technique of choice for the untargeted elucidation of aroma profiles, in foods and drinks, is one-dimensional gas chromatography, hyphenated to a mass spectrometer. It is obvious that GC–MS approaches can give qualitative (and possibly quantitative) information, but nothing on the odour sensation generated by a specific analyte. However, one of the main problems related to the 1D GC analysis of aromas is that such samples are excessively complex for a single GC column. The main consequence of insufficient separation power is that, often, compounds co-elute at the column outlet. In the present report, a head-space (HS) SPME-GC×GC–FID/MS method was developed for the analysis of Marsala wine. The FID trace was exploited for quantification purposes, while the MS data was used for identification.
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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).
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Identification of Phospholipid molecular speices by Neutral Loss Survey and MS3 Analysis
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Analysis of artificial colorants by ultra-fast liquid chromatography-mass spectrometry
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Analysis of Polyphenols in Green Tea using the LCMS-IT-TOF
The polyphenols or catechins in green tea are known to possess many health benefits for individuals. These species possess antioxidative activity and are also thought to have chemopreventive effects against certain cancers. The antioxidative activity of catechins is theorized to help improve hypertension, reduce inflammation, and improve cognitive dysfunction in the elderly all of which are beneficial to one’s health. The analysis of this class of compounds will continue to gain in importance as more individuals and companies (particularly those in the nutraceutical industry) discuss their potential health benefits.
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Multi-Dimensional Fragmentation of Anthocyanins from Rose Petals by Ion Trap – Time-of-Flight (IT-TOF) Mass Spectrometry
A Shimadzu high performance liquid chromatography – ion trap – time of flight mass spectrometer (LCMS-IT-TOF) was used to aid in the identification of anthocyanin species in rose petals. The effects of varying the parameters which control the collision energy and the collision gas were observed on cyanidin-3,5-diglucoside and its related mono-glucoside and anthocyanidin fragment signals. Further variation in these parameters were used to optimize iterative multi-stage fragmentation (up to MS6 ) in order to elucidate the fragmentation pathway of cyanidin-3,5-diglucoside.
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Quantitative Determination of Bisphenol A from Human Saliva using MAYI Trap column and LCMS – IT-TOF
The use of bisphenol A (BPA) has been a central topic amongst heated discussions on environmental toxicity. It is present in epoxy resins used in the sealants of canned foods, as a monomer unit of polycarbonate polymers, and as a plasticizer in certain polyvinyl chloride polymers, all of which has led to an increased chance of exposure. Despite a wide body of studies, which report the potential health risks associated with BPA exposure, the actual repercussions are inconclusive. Regardless, a growing need for fast, accurate methods to detect and quantify trace amounts of BPA from biological fluids to assess the validity of arguments from cases presented by both sides of the debate.
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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.
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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%.
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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.
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LCMS-8030/8040 Application - A study of the influence of collision cell design on the fragmentation of cathinones by LCMSMS (Austrailia)
Glyphosate is a widely used herbicide and residues in food and water for human consumption are of regulatory interest. The LCMS analysis of residual glyphosate and its metabolite AMPA in agricultural specimens is limited primarily by the impact of the polarity of these compounds on chromatography and sample preparation. We describe here the analysis of FMOC derivatised analytes using a reversed-phase separation and multiple ion MRM detection in negative ion ESI.
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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.
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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.
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LCMS-8030/8040 Application - Screening and Individual Quantitative Works of Regulated Substances in Food Using Triple Quadrupole Mass Spectrometer LCMS-8030 (Japan)
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.
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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.
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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.
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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.
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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.
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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.
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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”.
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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.
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LCMS-8050 Application - Simultaneous Ultrafast Analysis for Research of Anti-Cancer Drugs (SSI)
Mannitol possesses characteristics that include low moisture absorption and low reactivity, and is therefor used as an excipient for pharmaceuticals. USP methods for D-mannitol were amended in 2014 to specify the use refractive index detection with a 7.8mm x 300mm L19 column. The RID-20A differential refractive index detector features an optical system with dual temperature control to absorb the impact of subtle changes in temperature, thereby permitting chromatograms to be generated with a stable baseline. Here, we introduce an example of mannitol analysis using the RID-20A
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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
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LCMS-8060 Applicaiton - Enhancing ion sampling effciency, ion transmission and detection on a triple quadrupole platform (Japan)
Recent developments in triple quadrupole mass spectrometry have delivered higher sensitivity, lower detection limits and faster data acquisition speeds generating enhanced data quality. To further improve peak area response and higher sensitivity, the ion sampling efficiency, transmission and detection on a high-end triple quadrupole MS/MS system LCMS-8050 was modified whilst still supporting a fast polarity switching time of 5 ms and data acquisition speeds of 30,000 u/sec.
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LCMS-8050 Application - Direct Determination of Trace Hormones in Drinking Water by Large Volume Injection (UK)
In this study, the LCMS-8050 triple quadrupole mass spectrometer was used for the highly selective and sensitive detection of hormones in water to meet the requirements of UCMR3. This direct high volume injection method of analysis avoids the disadvantages associated with extracting samples using SPE as is commonly performed. Ammonium fluoride as an aqueous mobile phase additive was found to significantly improve response for all studied hormones in comparison to ammonium hydroxide. The excellent sensitivity of the final method provided detection limits ranging from 0.005 ng/L (testosterone) to 0.330 ng/L (17-α-ethynylestradiol).
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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.
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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.
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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.
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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.
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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.
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LCMS-8050 Application - High-Speed Analysis of Mycophenolic Acid in Plasma Using Triple Quadrupole LCMSMS (LCMS-8050) (Japan)
Mycophenolate mofetil is an immunosuppressive drug used to treat a refractory rejection after renal transplantation. 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.
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LCMS-8050 Application - High-Speed Analysis of Voriconazole in Plasma Using Triple Quadrupole LCMSMS (LCMS-8050) (Japan)
Voriconazole is a triazole antifungal agent that is used widely for the treatment of infections by fungi of the genus Aspergillus and Candida. This article introduces an example of high-speed analysis of voriconazole 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.
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LCMS-8050 Application - High-Speed Analysis of Itraconazole in Plasma Using Triple Quadrupole LCMSMS (LCMS-8050) (Japan)
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 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
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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).
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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.
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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.
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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.
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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.
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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).
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LCMS-8050/8060 Application - Enhancing Ion Sampling Efficiency, Ion Transmission and Detection on a Triple Quadrupole Platform
Recent developments in triple quadrupole mass spectrometry have delivered higher sensitivity, lower detection limits and faster data acquisition speeds generating enhanced data quality. To further improve peak area response and higher sensitivity, the ion sampling ef#31;ciency, transmission and detection on a high-end triple quadrupole MS/MS system LCMS-8050 was modi#31;ed whilst still supporting a fast polarity switching time of 5 ms and data acquisition speeds of 30,000 u/sec.
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LCMS-8060 Application - Oxysterol, Secosterols, and Cholesterol Intermediates Separation and Quantitation using Triple Quadrupole Mass Spectrometry
Monitoring oxysterol levels has become increasingly popular, as potential links between oxysterol levels and certain neurodegenerative disorders (such as Alzheimer’s disease, Parkinson’s disease, and multiple sclerosis) as well as various types of cancers are being explored. To meet the increasing research demand, a LCMS oxysterol separation and quantitation method was developed using a Shimadzu LCMS-8060 liquid chromatography triple quadrupole mass spectrometer.
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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.
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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.
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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.
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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.
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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.
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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%
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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.
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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.
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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.
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Using the LCMS IT TOF to identify impurities in pharmaceutical candidates using high mass accuracy
In the development of pharmaceutical candidates it is critical to identify by-products of the reaction mixture. In this paper we describe the application of a novel hybrid instrument platform delivering high mass accuracy data and MSn analysis in identifying impurity products from a relatively impure pharmaceutical candidate.
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HPLC Application - Improved R & D Efficiency Through Speedier Method Development (2) (Japan)
In LCMS measurement, the ionization mode is selected depending on the polarity of the target compounds. For example, Electrospray Ionization (ESI) is generally selected for analysis of high-polarity compounds which are typically found in drugs and pesticides, while Atmospheric Pressure Chemical Ionization (APCI) is selected for compounds having lower polarity
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Dual Ion Source DUIS-2020 for Simultaneous ESI and APCI Measurement
Since the LCMS-2020 utilizes the standard ESI probe as an integral component, upgrading to the DUIS-2020 is simple and cost efficient. Only a corona needle and secondary high voltage power supply need be added to allow simultaneous and continuous ESI and APCI analysis.
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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.
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Setting Optimum Dwell, Pause, and Scan Event Times on the Shimadzu LCMS-8030
Dwell, pause, and event times are important instrument settings that determine the exact amount of time the instrument monitors or scans for a particular event. Setting proper dwell, pause, and event times is necessary to achieve the best quality and quantity of data possible.
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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.
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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.
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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.
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Development of a Comprehensive Detection Method of Eicosanoids and Platelet Activating Factor Using Ultra-High Performance Liquid Chromatography/Mass Spectrometry
Using LCMS-8040, simultaneous detection method of eicosanoids and PAF was developed. 54 MRM transitions for 50 eicosanoids and PAF (platelet activation factor) were optimized. Limit of quantitation for several targets was in the subpicogram range.
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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.
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Metabolite Profiling of NSAID Effects In Vitro Using Shimadzu LCMS-IT-TOF System With Phenomenome ProfilerTM Software
Global metabolite profiling software was used to measure and compare the metabolic changes induced by several NSAIDs in HT29 cells and media. This approach can be used as a model system in monitoring drug metabolism in vitro. To help find components of biological significance the Shimadzu LCMS-IT-TOF was used to provide high mass accuracy MSn data integrated with Phenomenome Profiler software to integrate chromatography and mass spectrometry data sets together with statistical methods.
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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.
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LCMS-8030/8040 Application - Structural Analysis of 26 Pharmaceutical Compounds Using Synchronized Survey Scan Measurement (Japan)
Ultra Fast Speed: Fusion of Ultra Fast MRM and Ultra Fast Polarity Switching An Ultra Fast Scan Speed of 15,000 u/sec 500 MRMs per Second, the Most Ever Possible. High Reliability: Robust System Provides Long-term Data Stability UFsweeperTM Technology Dramatically Minimizes Cross Talk Excellent Linearity with Wide Dynamic Range. User-Friendly: Easy Maintenance for Minimized Instrument Downtime Single-vendor Solution Provides Seamless Operation Quantitation Browser for Effective Multi-analyte Quantitation.
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LCMS-2020 Application - Impurity Analysis of Highly-Polar Compounds Without Using Ion-Pair Reagents (Japan)
Here we introduce an example of flameless atomic absorption analysis of tap water spiked with cadmium at 1/10 the concentration specified in the revised ordinance, using the certified river water reference material JAC 0302 (spiked) provided by The Japan Society for Analytical Chemistry. In addition, the convenient automatic dilution and re-analysis function is introduced.
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LCMS-IT-TOF Applications - Profiling Analysis of Polysulfide Silane Coupling Agent (Japan)
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.
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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.
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LCMS-8030/8040 Application - Protein and Peptide analysis (SSI)
In an MS method, several events, such as MRMs and Scans may be selected. During acquisition, the instrument collects a data point for each MS event in sequence. After collecting a data point for each event, the cycle repeats and the instrument collects another data point for each MS event. The terms Loop Time, Cycle Time, and Duty Cycle all refer to the total amount of time necessary for the instrument to acquire one data point for each MS event in the method, including any time necessary to switch polarities or pause between events.
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LCMS-8030/8040 Application - Steroids: Testosterone, Progestrone, Estradiol, Ethinylestradiol (SSI)
Shimadzu’s High Salt Kit (P/N 638-93176-01 & 638-93176-02) will allow 12 times more sample injections on to the catalyst before replacement and increase the quartz combustion tube life by a factor of five. This type of kit is available for laboratory TOC-L or on-line TOC-4110 (P/N 638-93176-00) analyzers.
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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.
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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.
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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.
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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.
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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.
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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.
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LCMS-IT-TOF Application - Identifying changes in ethanol metabolism and endogenous metabolic profiles following the administration of alcohol as a liquid diet to mice (UK)
High-speed injections significantly improve throughput in multi-sample processing. Recently, a high-speed autosampler was introduced that features an injection time of just 7 seconds and an analysis cycle of 14 seconds. The combination of this autosampler with a high-speed quadrupole that features a positive/negative ionization switching time of 15 msec and a high-speed scanning rate of 15,000 u/sec was tested under ultra-high throughput conditions of four analytical runs per minute.
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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.
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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) .
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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.
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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.
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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.
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LCMS-8040 Application - Determination of 20 Phthalic Acid Esters in Alcoholic Drinks by Ultra High Performance Liquid Chromatography/Tandem Mass Spectrometry (China)
Thyroid hormones are essential hormones involved in growth regulation and development. Free circulating thyroxin concentrations are constant and are correlated with the tissue hormone level. Highly sensitive and specific methods are needed because most circulating thyroid hormone is bound to plasma proteins and only a few pg/mL are in the unbound free form.
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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.
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LCMS-8040 Application - Sensitive Assay of Free Thyroid Hormones by online SPE-UHPLC-MS/MS in Human Plasma (France)
Mycotoxins are contaminants in grains. For consumer food safety, quality control of food and beverages has to assay such contaminants. Rapid determination of the presence and then quantification of hazardous mycotoxins is essential. UHPLC-MS/MS offers the best combination of selectivity, sensitivity, and speed for detection of these compounds in complex matrices. In this study, a high throughput method for the quantification of 25 mycotoxins in various matrices was established
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LCMS-8040 Application - Micro-Flow UHPLC-MS/MS in Pesticide Analysis of Infant Foods (UK)
Tobacco specific nitrosamines (TSNA) are volatile compounds formed from nicotine and related alkaloids found in tobacco and tobacco products. The TSNAs are created during fermentation, curing and burning of the tobacco leaf. Due to their carcinogenic properties, the four major TSNA are assayed to control tobacco quality and to control cigarette smoke or public atmospheres.
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LCMS-8030/8040 Application - Identification and Quantitation of Degradation Products in Corn Stover Hydrolyzate for the Biofuels Industry (SSI)
Absinthe is an anise-flavored, distilled alcoholic beverage that was vilified and banned in many countries before the first World War. It was targeted because the beverage was alleged to have hallucinogenic effects; with the compound thujone thought to be the culprit. By the 1990’s, the advent of new food safety laws and a renewed interest in absinthe led to a lifting of the ban in many countries, but in some areas legal limits on thujone levels remain. In order to comply with food and beverage safety laws, a rapid and accurate measurement of thujone in absinthe is required. To accomplish this, a UHPLC-MS-MS method meeting these requirements of selectivity, sensitivity, and speed was developed.
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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.
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LCMS-8030/8040 Application - Drug Panel High App News for Customers (SSI)
Improving sample quality, throughput and reproducibility is of highest concern for clinical research; however, in order for progress to occur, it will be necessary to investigate new analytical strategies. This presentation will focus on an ultra-fast-immuno-MS platform that combines next-generation plasma separator cards with fully automated immuno-affinity and rapid digestion with reversed phase liquid chromatography coupled directly for mass spectrometric analysis.
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LCMS-8050 Application - A Rapid and Reproducible Immuno-MS Platform from Sample Collection to Quantitation (SSI)
To investigate the TOC in soils or other solids such as sediments or sludges, a solid sample module is used which enables TOC determination using the difference method and the NPOC method. Here, a subsample of the dried solids is weighed into a ceramic boat and combusted at 900 °C in a stream of oxygen. To ensure complete conversion to CO2, the generated gases are passed over a mixed catalyst (cobalt/platinum) for catalytic postcombustion.
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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.
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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.
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LCMS-IT-TOF Application - Development of Compound Identification Technique for Conjugated Unknown Compounds using Ion Trap Time of Flight Mass Spectrometry (Japan)
This work demonstrates the effectiveness of the iDplus platform for rapid differentiation of dairy products and identification of fraudulent practices. Proof of principle of this technique is demonstrated using milk profiling from several different species. The established method is then applied to foodstuff authentication using mozzarella cheese as a model product.
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LCMS-8050 Application - Accelerated and Robust Monitoring for Immunosuppressants using Triple Quadrupole Mass Spectrometry (Japan)
Nowadays, food and drinks are always a hot topic of discussion and in the focus of ‘state of the art’ analytical techniques. Food scandals all around the world from eggs to horsemeat, tainted wine, oil, and milk force the European Community to establish an integrated approach to food control. The target is a high level of food safety, animal health, animal welfare and plant health within the European Union through so-called ‘farm-to-table’ measures and monitoring, ensuring the effective functioning of the European market.
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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.
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LCMS-8040 Application - Determination of Benzimidazole Residues in Animal Tissue by Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry (China)
Recently, advanced oxidation processes (AOPs) have been used in water or wastewater treatment plants to further reduce trace pollutants and pathogenic microbes. Although these AOPs are believed to have the potential to mineralize residual pharmaceuticals in water, they often result in the generation of transformation products (TPs) that are structurally altered but are not further degraded. In some cases, these TPs are more toxic than parent compounds and hence contribute to the toxicity risk. Therefore, identification of the oxidized TPs for a variety of pharmaceuticals has recently attracted attentions. In this study, oseltamivir phosphate (OP) has been oxidized using ozone to identify the intermediates from the reaction.
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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.
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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."
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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.
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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.
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LCMS-8040 Application - Single Step Separation of Plasma from Whole Blood Without the Need for Centrifugation Applied to the Quantiative Analysis of Warfarin (UK)
We couple Noviplex cards for the isolation of small molecules from hydrolysed urine, with UHPLC and Ultrafast-LCMSMS (UFMS) to detect low level drug residues and metabolites in small volume biological specimens with subsequent identification of unknowns using MS scan events.
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LCMS-8050 Application - The Application of UHPLC and Ultrafast-LCMSMS to the Analysis of Small Volume Biological Samples for Drug Residues (Austrailia)
This application note presents instrument configuration, operating parameters, and analytical results for analysis of trace levels of 47 pesticides of various chemical classes in four orange oil samples using the Shimadzu GCMS-TQ8030 triple quadrupole GC-MS/MS. Results were evaluated for calibration linearity, analytical precision, sensitivity, and specificity.
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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.
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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.
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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).
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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).
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LCMS-8040 Application - Determination of Methamphetamine in Human Hair by Ultra High Performance Liquid Chromatography/Tandem Mass Spectrometry (China)
Methamphetamine is a neurotoxin and potent psychostimulant of the phenethylamine and amphetamine classes that is used to treat attention deficit hyperactivity disorder and obesity. Long-term use of methamphetamine can reduce dopamine activity in the brain. And substituted amphetamines abuse, such as methamphetamine, may cause lots of social problem. In public security system, blood and urine sample were collected usually to detect the narcotics level of the abuser. However, it is difficult to sample from the uncoordinated abuser. Hair sample can be used to detect the level of the methamphetamine as well as to conjecture abuse period.
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LCMS-8050 Applicatiion - Quantification and Structural Characterization of Glycans and Glycopeptides by TQMS: The Energy-Resolved Oxonium Ion Monitoring (Erexim) Platform (Japan)
Here we have developed new software to fully support Erexim data acquisition and analysis. Moreover, we acquired the Erexim profile database using purified glycan standards to enable glycan structure identification by pattern matching. The Erexim platform thus gives solution to both structural characterization and quantitative analysis of glycan and glycopeptides.
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LCMS-8050 Application - Fast and Sensitive Analysis of Drug Residues in Water Using on line SPE-UHPLC-MS/MS with Ultra-Fast Polarity Switching (France)
A fast and sensitive method was set up to assay a large number of drug residue in water. Limits of quantification are ranging from 0.1 to 5 ng/L with only 1 mL of sample and an automated sample preparation. Most of the compounds do not suffer from matrix effect without using internal standards. Some investigations are running to improve accuracy using selected internal standards.
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LCMS-8050 Application - Comparison of Matrix Effects in Multi-Residue Pesticide Analysis when using Online SPE or Direct Injection in Liquid Chromatography-Tandem Mass Spectrometry (France)
The aim of this study was to develop and compare two fast, sensitive and simple methodologies for the multi-residue of pesticides, that require the online SPE or direct injection in Liquid Chromatography-tandem Mass Spectrometry, thus the limits of quantification and matrix effects can be compared.
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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.
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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.
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Simultaneous Analysis of 97 Primary Metabolites By PFPP: Pentafluorophenylpropyl Column
A new method using a Pentafluorophenylpropyl (PFPP) column has been developed to overcome these limitations. This data sheet presents the simultaneous analysis of 97 primary metabolites, such as amino acids, organic acids, nucleotides, nucleosides and co-enzymes, using a PFPP column, which uses particles functionalized with a pentafluorophenylpropyl group. It allows not only hydrophobic interaction but also retention of hydrophilic compounds, which is essential for successful analysis of primary metabolites.
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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.
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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).
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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%.
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LCMS-8050 Application - Development of Automated Screening and Quantitation Approach on Movel On-Line SFE-SFC-MS/MS Platform- (I) For 23 Restricted Perflurocompounds in Textiles (Singapore)
In this study, a new analytical approach on the novel SFE-SFC-MS/MS platform was developed for analysis of 23 PFCs including PFOA and PFOS spiked in textiles. The results indicate that the new approach is potentially possible for screening and quantitation of targeted analytes in un-pretreated solid samples directly. The detection sensitivity of the 23 PFCs spiked in clothing sample achieved is at the level of 25 pg or 0.42 µg/kg. However, validation of the SFE-SFC-MS/MS approach for actual samples are not carried out yet.
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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
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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.
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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.
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LCMS-8060 Application - Full automated online sample extraction and analysis of mycotoxins in foods by online SFE-SFC-MS (SSI)
Mycotoxins are low-molecular-weight natural products produced by fungi and are capable of causing disease and death. They are strictly regulated around the world because of their strong carcinogenic effects. A simple and reliable method to analyze mycotoxins is required to ensure food safety. The current methods require time-consuming sample pretreatment. Here we report a fully automated online sample extraction and analysis of mycotoxins in foods by online SFE-SFC-MS.
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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.
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LCMS-8060 Application - Automated Screening of Explosives in Soil Samples by Online SFE-SFC-MS (SSI)
There are a large number of explosives-contaminated sites in the US, Europe, and Asia. High levels of explosives in soil can threaten the health of humans, livestock, and wildlife. A number of remediation efforts are underway, which require the analysis of explosives in soil samples. Recently, a new technique was introduced that allows the automated supercritical uid extraction and SFC analysis of explosives in soil samples with minimal sample preparation and handling requirements to save analyst time and sample preparation expenses.
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LCMS-8050 Application - Development of MRM assay for the determination of potential biomarkers in case of severe vivax malaria (India)
Plasmodium vivax malaria has the most widespread global incidence and its diagnosis, treatment and control is much more challenging than P. falciparum malaria. P. vivax can cause severe and fatal manifestations even at a very low parasite biomass. However, there is no precise, systematic global assessment of endemicity for vivax malaria. Vivax malaria is no more considered benign; causes of its severity and the associated mechanism still remains obscure. In this study, serum samples from patients diagnosed with Severe Vivax Malaria (SVM) and Healthy Controls (HC) from different endemic regions of India were investigated using quantitative MRM approach.
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LCMS-8060 Application - Phospholipid profiling by two distinct MRM measurements to identify phospholipid's class and fatty acid composition (Japan)
The role of phospholipids in vivo has a wide variety of functions such as the structural units of the cellular membrane, the storage and transport of lipids in the blood, the precursor of the lipid mediators and the energy source. To understand the role of phospholipids in the biological functions, quantitative analysis for the phospholipid composition ratio in the blood and tissues becomes an important indicator. Here we developed the analytical workflow to comprehensively analyze the major phospholipids in vivo by combining two distinct MRM measurement.
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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.
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LCMS-8050 Application - Simultaneous Quantification of Tryptophan-related Metabolites as Biomarkers for Prediabetes (Japan)
To identify biomarkers for prediabetes, we recently performed a longitudinal study of changes in plasma metabolites using two different rat models of type 2 diabetes (T2D), the SDT rat and the OLETF rat, and found that the metabolites in tryptophan metabolism (tryptophan and kynurenine) were decreased at prediabetic state in both rat models, suggesting that tryptophan and its metabolites are potential biomarkers for prediabetes.
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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.
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LCMS-8060 Application - Ultra-sensitive and rapid assay of neonicotinoids, fipronil and some metabolites in honey by UHPLC-MS/MS (France, EU)
Neonicotinoids are a class of insecticides widely used to protect fields as well as fruits and vegetables. Recently the use of this 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 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.
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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.
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LCMS-8060 Application - Automated Screening of Explosives in Soil Samples by Online SFE-SFC-MS
There are a large number of explosives-contaminated sites in the US, Europe, and Asia. High levels of explosives in soil can threaten the health of humans, livestock, and wildlife. A number of remediation efforts are underway, which require the analysis of explosives in soil samples. Recently, a new technique was introduced that allows the automated supercritical #31;uid extraction and SFC analysis of explosives in soil samples with minimal sample preparation and handling requirements to save analyst time and sample preparation expenses.
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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.
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LCMS-8060 Application - Phospholipid Analysis using SimLipid Software (Japan)
Here we shows the analyzing results by LCMS-8060 of phospholipid changes in a liver tissue between a control and a mouse which a fluorescent probe has been administered by a tail vein injection. In this analysis, SimLipid software from PREMIER Biosoft, USA was used to estimate the candidate of PLs fluctuated between a control and a probe administered mouse.
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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.
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LCMS-8050 Application - A Rapid LCMS Method for Evaluating PPCPs Contaminants Found in Drinking Water
A robust and rapid 6.5 minute method for evaluating pharmaceuticals and personal care products was developed using ultra-fast liquid chromatography mass spectrometry. Most analytes had an lower limit of quantitation at a level between 0.1 ppb and 5 ppb. Miconazole was the only drug detected in the river water samples. The samples may have been too diluted from the excessive amount of rain in the area before sampling occurred. The method can be used to further test other river water samples when there is a more stable water table to test from.
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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.
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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
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LCMS-IT-TOF Application - Assessing metabolic profiles in chimeric PXB mouse with humanized livers following oral dosing of troglitazone (UK)
Changes in endogenous metabolites through ethanol administration has enabled a greater understanding of metabolic stress responses. Alcohol can be delivered via intragastric cannulas or through liquid diets in which animals can be given alcohol for several months and high blood alcohol levels can be maintained. However, in this study a less invasive, four week ethanol enriched liquid diet model was evaluated as an alternative vehicle. To assess the impact of reduced level ethanol exposure, a systems based approach was taken measuring urine, plasma and liver tissue to characterize both ethanol metabolites and endogenous lipid changes. Samples were measured by liquid chromatography ion trap mass spectrometry (LCMS-IT-TOF), separated by Nexera UHPLC. Metabolite identity was confirmed via the combination of accurate mass formula prediction, authentic standard analysis and database searching (LipidMaps, Metlin, HMDB and KEGG).
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LCMS-8030/8040 Application - Development of an ion transmission enhanced tandem ion guide system for triple quadrupole mass spectrometer (Japan)
Antipsychotic and atypical antipsychotics are used to treat a wide variety of psychiatric conditions such as schizophrenia, acute mania, bipolar disorder, and depression. Recently a high number of children are being treated with antipsychotics for emotional or behavioral disorders. Therapeutic drug monitoring is in demand due to the risk of toxicity, unwanted side effects, and potential pharmacokinetic interactions. Additionally, a co-administered drug can potentially inhibit or induce the metabolism of the antipsychotic drug such as antibiotics, selective serotonin reuptake inhibitors, cigarette smoking, and barbiturates. 1 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.
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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.
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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.
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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.
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LCMS-IT-TOF Application - Online Study on Metabolites Profiles of Sixteen Clausenamide Enantiomers In Vitro by Liquid Chromatography/Quadrupole Ion Trap/Time of Flight Mass Spectrometry (China)
Industrial dyes is a class of dyes which has been widely used in the production of textile, fur and leather, wood and china, which using as food additive is forbidden because of potential toxic effects. Industrial dyes illegally added in food were reported frequently, therefore departments like China FDA focused on the determination of industrial dyes in food, and they needed to develop a quick, high sensitivity and high accuracy qualitative and quantitative method. The food samples were extracted by a mixed organic solution, cleaning up on an SPE column, then the extracts were analyzed by LCMS-IT-TOF. In this study, 10 basic industrial dyes and 9 acidic industrial dyes in food were analyzed. External standard method was used for quantitative analysis, and MSn (n>2) results were used for qualitative analysis.
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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.
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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.
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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.
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Perfinity and LCMS-8050 Application - Quantitative Analysis of IGF-1 Using Online Digestion Coupled to the Triple Quad LCMS-8050 (SSI)
The SmartPrep Extractor, using new Supel Tox DON SPE cartridge technology, efficiently prepared a variety of wheat samples representing the agriculture and processed food chain prior to HPLC analysis. Sample matrices representing the food chain (unprocessed cracked wheat, unprocessed wheat berries, processed natural wheat germ, consumer shredded wheat cereal, and consumer infant whole wheat cereal) were selected for this application. Data presented concludes that deoxynivalenol is effectively recovered using automation from a variety of samples with and without natural deoxynivalenol present. Recoveries for all matrices meet both United States and European Union limits.
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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.
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LCMS-8060 Application - Development of simplified quantitative method for tryptic digested C-reactive protein by using online SPE coupled to LCMS/MS (Japan)
Method development for accurate quantification of biomarker protein is very important step for the researchers in pharmaceutical industries and clinical fields. Mass spectrometry based quantitative proteomics approach shows a big potential to be the substitution of ELISA due to its precision, accuracy and multiplexing capability. In order to achieve the required sensitivity and selectivity, nano scale liquid chromatography mass spectrometry or sample preparation method including depletion of dominant protein and/or enrichment of target protein are frequently used. In this study, we tried to develop simple and high sensitive quantification method for C reactive protein (CRP), the level of which rise as a result of inflammation etc., by using online SPE coupled to triple quadrupole mass spectrometer without any complicated sample enrichment and depletion.
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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.
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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.
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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).
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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.
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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.
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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).
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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GCMS-TQ8030 Application - GC/MS/MS Analysis of Pesticides in Drinking Water (Japan)
The SAMHSA drugs of abuse panel requires confirmation of 11 compounds in urine by either gas or liquid chromatography with mass spectrometery. Methods for these compounds have been developed using the LCMS-8030 and LCMS-8040 consistent with the SAMHSA guidelines for method performance and validation.
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LCMS-8040 Application - Strategies for Structure Elucidation Using Ultrafast Mass Spectrometry (UFMS): Using nMS2 as an Alternative to MS3 (Austrailia)
A triacylglyceride (TAG) is an ester derived from glycerol and three Fatty Acids (FA). TAGs are found in both plant oils and animal fats. Different varieties of oils are used for culinary purposes across the globe. Hence, their characterization is important for nutritional reasons. However, separation and identification of components of the complex mixtures of TAG that constitute fats and oils is a challenging. Characterization of the TAGs present in edible oils requires acquisition of precursor ion m/z by full scan MS mode. Full scan MS spectra are generally complicated because of presence of varieties of TAGs. Furthermore, it is necessary to fragment all these precursor ions so as to understand fatty acid composition of TAGs. Selecting these precursor ions manually and creating a method to fragment them is also a tedious task. This task is simplified by Synchronized Survey Scan (SSS) available in LCMS-8040 with LabSolutions software. Here, product ion spectra of all the major precursor ions are obtained as a dependent event of full scan MS in a single analysis, attributed to ultrafast scanning speed of 15000 u/sec of LCMS-8040.
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LCMS-8050 Application - Cooked Meat Product Analysis by LCMS/MS to Determine Between Animal Species Using Proteotypic Peptide Quantitative Proteomic Analysis (UK)
With the emergence of new food safety challenges innovative analytical technologies are being developed to enable industry stakeholders and regulators to make sound scientific decisions. These advances have been made in response to changing regulations and needs and also to help maintain the safety of the food chain. In the case of unwanted or undeclared ingredients food authenticity testing is important component in many quality and safety programs. In 2013, horse meat issues received intense scrutiny and Polymerase Chain Reaction (PCR) techniques were used to screen for horse DNA in processed food samples. However, despite its widespread use in Europe for food fraud, PCR is problematic. DNA extraction kits are expensive and often require up to 8 h for the extraction, followed by cleanup and the PCR process. DNA is also prone to degradation especially in processed food. In contrast, mass spectrometry enables a promising approach to the detection of marker peptides in tryptic digests of horse, pig, beef and chicken with high sensitivity. 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 Uniprot database FASTA download for myosin (43263 proteins) and collagen (44531 proteins) to determine no other species cross reactivity to pig myosin and collagen.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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LCMS-IT-TOF Application - Automated Compound Identification Using Product Ion Scanning with Accurate Mass Measurement and Compound Database Searching for Non-Targeted Metabolomics (Japan)
Glycerophospholipids (GPLs) are the major components of biological membranes. Not only can GPLs act as a barrier from outer environment, but also they play a key role in a variety of biological processes including membrane trafficking, signal transduction, and so on. Thus, analysis of GPLs is one of the most important studies in metabolomics field. Although ESI-MS coupled with RP-HPLC is an effective strategy for lipidomics, it is necessary to further improve analytical methods. One drawback to perform comprehensive identification and precise quantification of minor species of GPLs using ESI-MS is interference from matrices or other components. In order to solve this problem, we managed to establish a new strategy to analyze GPLs by using 2DLC-MS/MS, i.e. two-dimensional liquid chromatography coupled with triple quadrupole mass spectrometer.
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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.
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LCMS-8030 Application - Determination of the Derivatives of Nitrofuran Metabolites in Marine Products by Ultra High Performance Liquid Chromatography/Triple Quadrupole Mass Spectrometry (China)
Clausenamide is a chiral nootropic drug extracted from Clausena lansium (Lourd.) Skeels. It has been synthesized in the Institute of Materia Medica and has been studied in the clinical trials of Phase II. The nootropic effect of (-)-clausenamide is much better than that of (+)-clausenamide and the latter has stronger toxicity than the former. In addition, including the (-)-clausenamide and (+)-clausenamide, all clausenamide enantiomers have different effects on colony form frequency in human embryonic neural stem cells, and as well as on induction of LTP in hippocampal of rat, and on concentration of nerve cell cytosolic free calcium. The biotransformations of sixteen clausenamide enantiomers have been investigated in vitro in this study. The stereo-selectivity on metabolism and differences of sixteen clausenamide enantiomers has been elucidated by means of identification of metabolites and explanation of pathways.
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LCMS-8040 Application - Determination of Microcystins in Drinking Water by Ultra High Performance Liquid Chromatography/Triple Quadrupole Mass Spectrometry (China)
This poster describes a method by ultra high performance liquid chromatography/tandem mass spectrometry (UHPLC/MS/MS) to analyze 4 derivatives of nitrofuran metabolites in marine products. Thanks for the high sensitivity and selectivity of UHPLC/MS/MS method, determination of these compounds was successful. The limit of quantitation (LOQ) of AMOZ was 0.4 µg/kg, which is lower than the guideline value (0.5 µg/kg) proposed by the USFDA. The derivatives of nitrofuran metabolites used in breeding of marine products are known to have a carcinogenic effect. Quantities of these compounds in marine products were regulated by the USFDA. This paper describes a UHPLC/ESI-MS/MS method to determine 4 derivatives of nitrofuran metabolites. The method is simple, rapid and highly sensitive and meets the requirements.
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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.
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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.
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LCMS-8040 Application - Determination of 200 Residual Pesticides in Food by Ultra High Performance Liquid Chromatography/Triple Quadrupole Mass Spectrometry (China)
Phthalic acid esters (PAEs) are a group of commercial chemicals widely used to make plastics more malleable and help lotions penetrate skin. A number of phthalate esters are known to cause birth defects or reproductive harm. PAEs can migrate from plastic materials to the environment. They are often found in water, soil, air, food products and the human body. As well known, alcoholic drinks have always been popular around the world. In alcoholic drinks production, plastic containers are typically used in the storage and transportation process, which could make some phthalate esters leak easily from PVC tubes or vessels as well as plastic caps. The aim of this study is to determine the level of phthalate esters migration in alcoholic drinks by fast liquid chromatography-electrospray tandem mass spectrometry. This method is simple and rapid with acceptable sensitivity to meet the requirements for the analysis of PAEs in alcoholic drinks.
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LCMS-8040 Application - Rapid Simultaneous Assay of 23 Mycotoxines in a Variety of Food Sample by UHPLC-MS/MS Using Fast Polarity Switching (France)
Therapeutic drug monitoring (TDM) of antidepressants is one of the most widely utilized analysis in clinical labs in Dutch hospitals nowadays. Traditionally quantitation of antidepressants is performed by means of HPLC with diode-array detection (DAD). Obvious disadvantages of the latter method are: sensitivity, selectivity and possibility of false positives as a result of co-elution with other administered drugs, metabolites or endogenic compounds. UHPLC-MS/MS is much more sensitive, more selective, and if robust the perfect replacement of routine HPLC analysis. Due to simplified sample prep, faster analysis and less solvent consumption UHPLC-MS/MS is much more cost effective. UHPLC-MS/MS methods will replace routine HPLC methods in clinical labs.
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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.
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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}.
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LCMS-8050 Application - Accelerating Quantitative Proteomics Analysis with Shimadzu UFMS and Skyline (Japan)
Beta-agonists are a group of veterinary drugs that can be added to animal feed to work as growth promoters due to their ability to increase muscle mass and decrease fat deposition. However, due to their adverse effects to human health, these compounds have been banned for growth promoting purposes in farm animals by the European Union (EU Council Directive 96/22/EC) and other regulatory agencies worldwide. To support regulatory compliance a simple and rapid UHPLC-MS/MS method was developed for the reliable quantitation of beta-agonists in bovine urine and liver. To enhance data quality and reduce false positive reporting the method was optimized to acquire multiple SRM transitions for each compound and mass spectral library searching.
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LCMS-8040 Applicaiton - Simultaneous Analysis of 97 Primary Metabolites by PFPP: Pentafluorphenylpropyl Column (Japan)
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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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
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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.
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LCMS-8050 Application - Ultrafast and Robust Optimization of Peptide MRMs Using a Fast-Scanning Triple Quadrupole Mass Spectrometer (SSI)
Targeted proteomics methods may be composed of tens or hundreds of MRM channels corresponding to peptides from a wide variety of proteins of interest. Although precursor and product ions can be calculated in advance, the best ions for monitoring among all possible channels need to be selected and confirmed before analyzing a large or material-limited sample set. Similarly, collision energy and other instrument parameters may be estimated or modeled by software but require fine-tuning and verification to maximize instrument response for each channel. A fast-scanning triple quadrupole mass spectrometer has been used with proteomics software to verify and optimize large numbers of MRM transitions with a minimum number of optimization runs.
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LCMS-8050 Application - A Sensitive and Repeatable Method for Characterization of Sulfonamides and Trimethoprim in Honey Using QuEChERS extracts with Liquid-Chromatography-Tandem Mass Spectrometry (SSI)
The antibacterial sulfonamides (SA) and trimethoprim are widely used in veterinary and human medicine. Diverse foods from animals potentially contain residues of these drugs posing possible threats to people by triggering allergic reactions and undesirable increasing of microorganism’s drug resistance. Various countries have de ned their own maximum residue limits (MRLs) for sulfonamides accepted in honey, There are no MRL’s for sulfonamides in honey in the UE but in 2002 a minimum required performance level (MRPL) was set for analytical methods at a level of 10 µg/kg. HPLC-MS/MS is an effective strategy to characterize and accurately measure those antibiotics considering MRLs and MRPLs in food products from animal origin tend to be continually reduced to preserve human health safety. A selective, fast and sensitive HPLC-MS-MS method has been developed for 15 sulfonamides and trimethoprim.
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LCMS-8050 Application - Rapid, High Throughput Quantitation of Cyanotoxins in Natural Water by UHPLC-MS/MS (SSI)
Cyanotoxins are toxins produced by bacteria called cyanobacteria (also known as blue-green algae). Cyanobacteria are found in lakes and in the ocean where they can reproduce exponentially to form blooms. The most prevalent cyanotoxin is the hepatotoxin microcystin and it is a problem worldwide in freshwater ecosystems. The World Health Organization has set the guideline for permissible amount of the microcystin LR in drinking water at 1ug/L. The National Center for Environmental Assessment suggests a limit of 0.1 μg/L. Current EPA Method 544 requires solid phase extraction of 500 mL of sample, evaporation and reconstitution in 1 mL of methanol. This work demonstrates a quick screening method without the use of sample forti cation that greatly reduces sample prep time and meets detection requirements.
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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.
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LCMS-2020 Application - 3rd Party - High Speed Analysis of Explosives (EAS)
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. These columns provide faster chromatography results since they are able to run at higher linear velocities without a significant loss in column efficiency. However, the smaller particle sizes and required hardware may lead to clogging issues, especially with samples that may be contained in a difficult matrix. 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. Good resolution of fourteen explosives could be obtained within eight minutes. Results obtained by varying column dimensions to determine the effect on resolution will be presented along with a variety of detection techniques.
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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.
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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.
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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.
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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.
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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.
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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.
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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).
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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.
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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.
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LCMS-8060 Application - Multi-residue analysis of pesticides in agricultural products using QuEChERS and SFC/MS (Japan, SSI)
Analysis of pesticide residues in food is typically time-consuming due to the separation for multiple pesticides with a wide range of polarity and matrix co-eluting issues. To deal with the ever-growing number of pesticides, food safety laboratories need to ideally screen as many compounds as possible in a short time which may exceed maximum residual limits; typically 10 ppb in food matrices. Supercritical fluid chromatography (SFC) is one of the separation techniques, and it offers high resolution at high ow rates and various separation modes. Therefore, it has the potential to separate multiple pesticides in a single run. In this study, we developed an analytical method for 441 pesticides in food matrices by QuEChERS and SFC/MS.
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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.
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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.
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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.
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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.
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LCMS-8050 Application - Development of Automated Screening and Quantitation Approach on Novel On-Line SFE-SFC-MS/MS Platform- (II) for FIve Aflatoxins in Powdered Food Samples (Singapore)
Supercritical fluid chromatography (SFC) is one of the trendy analytical techniques in recent years. By using carbon dioxide (CO2) as eluent, the SFC has a number of advantages like environmental friendly, cost effective and suitable for a wide range of analytes’ polarities. The Nexera UC system (Shimadzu) is a further developed platform combining SFE (extraction) and SFC with MS/MS into a complete system to handle from sample pre-treatment and separation to superior MS/MS detection and quantitation in a fully automated manner. The novel SFE-SFC-MS/MS system has been used successfully for analysis of 510 residual pesticides in agricultural products. Here we describe the applications and advantages of the Nexera UC system in analysis of a atoxins (B1, B2, G1, G2 and M1) in powdered food such as corn our and wheat flour.
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LCMS-8060 Application - High sensitive analysis of peanut allergen in cumin and spice mix (SSI)
Food allergens are a major public health concern. Among them, peanut allergy is one of the common food allergies. To avoid unexpected contact with food allergens, food labels are strictly used to indicate the presence of specific allergens. With the increasing awareness of food allergies, the presence of undeclared peanut in cumin lead to huge recalls in recent years. Although ELISA is one of the commonly used technique to detect allergens, its false-positive rate is a major concern due to its cross-reactivity. We developed a method with high specificity and sensitivity to overcome this issue by using a high sensitivity triple quadrupole mass spectrometer to detect peanut allergen Ara h1 in commercially available spices and seasonings.
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LCMS-8060 Application - Pesticids analysis in complex food extracts by multi-transition MRM and library searching for enhanced residue confirmation (UK)
In this work, a conventional MRM method developed for routine pesticide analysis (typically monitoring 2-3 MRM transitions for each pesticide) has been modified and extended to include a higher number of MRM transitions specific to each pesticide compound (dependent on the pesticide in question, typically 6-12 fragment ions per-compound are monitored). This approach has not been possible on previous MS instruments due to the limited duty cycle resulting in shorter dwell times or an increased cycle time for each MRM and as a consequence lower peak sampling rates and lower sensitivity. Using a fast scanning triple quadrupole mass spectrometer this approach was applied to the routine analysis of a panel of 202 pesticides spiked into a matrix.
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LCMS-8050 Application - MRM based targeted analysis of serum samples to demonstrate differential expressed proteins in severe cases of falciparum malaria (India)
Malaria is a vector borne infectious disease caused by protozoan parasite Plasmodium spp. Plasmodium falciparum is major causative organism associated with malaria related morbidity. It is transmitted from one person to another via carrier female Anopheles mosquito. There are primarily four different species of Plasmodium (P. falciparum, P. vivax, P. malariae, and P. ovale), which generally infects animals. P. vivax and P. falciparum are most common malaria parasite species which cause malaria in human beings. Present study aims to validate potential protein markers, expressed differentially in severe (SFM), non severe (NSFM) falciparum malaria as compared to healthy control. MRM assays were employed to gain mechanistic insights into disease pathogenesis and host immune responses
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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.
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LCMS-8060 Application - Quantitative Multi Target Screening (MTS) using liquid chromatography-tandem mass spectrometry with MS/MS library based identification for forensic toxicology (MSO,SEG)
Multi Target Screening (MTS) has been applied to systemic toxicological analysis to reduce false positive and negative reporting using MS/MS spectral library based identification. MTS methods uses threshold triggered multiple reaction monitoring (MRM) and MS/MS product ion scans at three collision energies to confirm the compound identification based on mass spectral library searching. The MS/MS library was created using certified reference materials and included electrospray spectral data from over 1200 compounds relevant to clinical and forensic toxicology in both positive and negative ion modes. The MTS approach was applied to screening whole blood samples at three concentration levels to evaluate screening at therapeutic, overdose and toxic concentrations.
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LCMS-8050 Application - MRM-based assay for identification of potential protein biomarkers in Meningioma patients (India)
Meningiomas are tumors originating from meningeal layers of brain and spinal cord, comprising nearly 30% of the primary Central Nervous System (CNS) tumors. The 2007 WHO classification showed 15 histopathological subtypes of meningioma and 3 different histological grades namely the grade I, II and III. However, there is an enormous amount of heterogeneity among the grades thus pointing out to a need of grade specific biomarkers for diagnosis and better prognosis of the tumor. Molecular studies to decipher the molecular mechanisms for meningioma development and progression has pointed out involvement of tumor suppressors: TIMP1,TIMP3 among several others. Subsequently, proteomic alterations in meningiomas have also been looked into to identify the exact players that are involved in meningioma pathobiology. Hence, MRM based methodology was developed to study these potential protein biomarkers from meningioma patients post surgical resection so as to gain mechanistic insights for therapeutic intervention.
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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.
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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.
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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.
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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.
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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.
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LCMS-8060 Application - Multi-Component Analysis of Five Beers (Japan)
Sensory test methods that present flavor and taste in numerical terms are widely used techniques for the quantitative evaluation of food quality. Recently, attempts have been made to obtain a greater amount of data by combining the results of sensory tests with metabolomics data that provides a comprehensive analytical data with use of multivariate analysis has become an effective option for elucidating the differences in a wide range of constituents. This combination of multivariate analysis and metabolomics promises to see application in areas of quality evaluation and quality improvement, as well as in the development of foods with improved functional properties. In this article, we describe the simultaneous analysis of five commercially available beers with a triple quadrupole mass spectrometer (LCMS-8060) using a primary metabolite method package, and performing principle compnentn analysis on the data set obtained using TraverseTM MS software. We classified the five beers based on differences in constituent compounds, and confirmed characteristic components in each beer. We then performed hierarchical clustering analysis to show how these five beers are classified.
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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.
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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.
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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.
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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.
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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.
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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.
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LCMS-8050 Application - Analysis of 90 Multi-Class Drugs with Polarity Switching in Plasma (SSI)
Since medical marijuana (MM) was legalized in California in 1996, 23 states and Washington, D.C. have passed laws allowing its use for a variety of medical conditions. From a consumer safety point-of-view, quantitation of the pesticide residues in MM products has begun to attract wide interest. There are several problems associated with analysis of pesticide residues in MM. First and foremost, there are very few regulatory guidelines established to de ne which pesticides to include or what the detection limits should be, and secondly the matrix is very complex with significant interferences. Finally, sample load is growing exponentially, so the chosen method must be quick and easy to perform. Trace level pesticide analysis in complex food matrices have been done for many years with similar challenges, thus many of the analytical protocols emerging for the MM matrix are based on these well-established techniques. Triple-quadrupole GC-MS/MS operated in MRM mode provides significant sensitivity and selectivity, but method development can be expensive and time consuming. This poster describes streamlined method development process for analysis of pesticide residues in MM using a QuEChERS sample preparation method, followed by GC-MS/MS detection and quantitation.
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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.
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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.
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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).
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Natural Product Analysis Utilizing an Ion Trap - Time-of-Flight Mass Spectrometer (IT-TOF)
Recently, the popularity of remedies consisting of natural products found in foods, roots, and herbs has increased in both the domestic and global healthcare markets. As a result of this renewed focus on natural remedies, efficient identification and analysis of the active compounds in these products is a growing area of method development. The LCMS-IT-TOF allows researchers in this field to obtain both chemical and structural information as it utilizes both the fragmentation power of the ion trap and the high resolution, and mass accuracy, of a time-of-flight mass spectrometer.
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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>.
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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>.
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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.
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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.
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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.
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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.
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Quantitative Analysis of Veterinary Drugs Using the Shimadzu LCMS-8050 Triple Quadrupole Mass Spectrometer
Foods in which chemical residues, like pesticides, feed additives, and veterinary drugs found in excess of maximum residue levels have been banned from sale in many countries around the world. Compounds that are subject to residue standards vary widely and the list is expected to grow. Because of this, there is a need for a highly sensitive and rapid analytical technique to analyze as many of these compounds as possible in a single run. This Application News introduces an example of the high-sensitivity analysis of 89 veterinary drugs in a crude extract of livestock and fishery products.
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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).
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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.
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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.
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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.
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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.
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LCMS-8060 Application - 500 Years German Beer Purity Law – Searching Contaminants_Glyphosate_Metals_Shimadzu
Beer is made from natural grain and vegetable base products which are exposed to environmental impacts as well as agricultural treatment. Beer may therefore contain a variety of heavy metals such as arsenic, lead and cadmium and additional undesired substances such as mycotoxins and pesticides. To track and analyze these elements and compounds various analytical technologies and sensitive analytical systems are required. Shimadzu is offering the full solution such as UV-Vis spectrophotometers, atomic absorption-, ICPOES/MS spectrometers, liquid- and gas chromatography as well as mass spectrometry, and TOC analyzers to permanently guarantee the highest quality of the most popular alcoholic drink in Europe.
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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.
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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.
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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.
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High Sensitivity Analysis of Peanut Allergen in Cumin and Spice Mix [LCMS-8060]
Food allergens are a major public health concern. Among them, peanut allergy is one of the common food allergies. To avoid unexpected contact with food allergens, food labels are strictly used to indicate the presence of specific allergens. With the increasing awareness of food allergies, the presence of undeclared peanut in cumin lead to huge recalls in recent years. Although ELISA is the most commonly used technique to detect allergens, its false-positive rate is a major concern due to its cross-reactivity. We developed a method with high specificity and sensitivity to overcome this issue by using a high sensitivity triple quadrupole mass spectrometer to detect peanut allergen Ara h1 in commercially available spices and seasonings.
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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.
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LCMS-8060 Application - Developing a Chiral Amino Acid Analysis Method That Uses Column Switching (Japan)
Analysis of D-amino acids is susceptible to interference by a wide variety of peptides and amino compounds, and therefore requires high sensitivity and highly selective analysis methods for accurate measurement. Furthermore, conventional optical separation analysis of amino acids necessitated derivatization and long separation times of the amino acids. This article introduces a rapid analysis method that employs chiral columns to achieve high separation and high sensitivity and that dispenses with derivatization. This system uses two types of chiral columns alternately with high-pressure column switching valves (FCV) and allows fully automatic analysis of a wide range of D- and L-amino acids.
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LCMS-8060 Application - Phospholipid Analysis for Four Types of Mouse Tissues (Japan)
Here phospholipid analysis was performed by precursor ion scan (PIS) or neutral loss scan (NLS) with a triple quadrupole mass spectrometer for mice – derived brain, spleen, lung and liver tissues. In estimating candidate phospholipids, we performed the database search using SimLipid software from PREMIER Biosoft, USA. Phospholipids characteristic of each tissue were detected from four different tissue extracts and the effectiveness of the database search by SimLipid software was confirmed.
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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.
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LCMS-8050 Application -Vitamins in Milk Infant formula
Milk infant formulas are generally enriched with vitamins and complements which are essential for normal health and growth. The manufacturers must insure that their content is controlled properly. Also they must certify the absence of certain contaminants. Traditional methods to measure complements and contaminants in this matrices are based on HPLC thanks to the possibility of rapid separation and quantification. Mass spectrometry detection is the gold standard due to its specificity, precision and sensitivity. However, because of the high variability of structures and chemical properties of this analytes, several methods are needed for both their extraction and their separation by chromatography. We here report a unified solution for the quantification of all of this compounds in milk infant formulas.
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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.
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LCMS-8060 Application - Automatic, simultaneous and rapid analysis of 22 drugs of abuse in saliva by on line SPE and UHPLC-MS/MS
The drugs quantification of abuse in saliva offers information on the state of individual consumption by non-invasive and easy sample collection. Narcotic substances are detected in saliva from four different drugs family. Nevertheless, the concentrations of these drugs in saliva are lower than those found in blood or urine. Moreover, this analysis is based on the detection of parent compounds and not metabolites. Therefore, the analysis must be performed within 24 hours. So, it is necessary to use a very sensitive and rapid analysis method. The objective is to have a robust and automatic analytical method allowing the analysis of all these substances for hundred samples per day.
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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).
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LCMS-8050 Application - Pharmaceuticals and Personal Care Products (PPCPs) in Surface Water (SSI)
A robust and rapid 8 minute method for evaluating pharmaceuticals and personal care products was developed using ultra-fast liquid chromatography mass spectrometry. Most analytes had an lower limit of quantitation at a level between 0.25 ng/mL and 5 ng/mL. Amphetamine was the only compound detected in samples taken from the western part of the US. Samples from the Midwest and the eastern part of the US did not test positive for the reported compounds.
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LCMS-8060 Application - Sensitive and Fast Measure of Aminoglycoside Antibiotics in Milk, Meat, or Eggs by HILIC-MS/MS and Identification using MRM Spectrum Mode
A very sensitive HILiC-MS/MS method was developed to detect a large panel of aminoglycoside antibiotics without ion-pairing. One method can be used for all kind of animal species or commodities, covering major food safety regulations. The complete work flow, including sample preparation has been optimized to provide high-throughput. The good recoveries obtained across the tested matrices eliminate the use of matrix-matched calibration standards. In addition to the fast quantitative screening method, a ID confirmation method using MRM Spectrum Mode can be performed with same mobile phases and column.
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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.
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LCMS-8050 Application - Simultaneous analysis of major allergens in food matrices by high sensitive mass spectrometer
Recently, liquid chromatography mass spectrometry becomes an alternative technique to detect allergenic proteins with high selectivity, sensitivity, and capability to analyze multiple allergens simultaneously. We developed a method to detect 31 peptides derived from eight allergens. We analyzed commercially available samples such as bread and gluten free bread etc to evaluate this method. We did not detected any peptides derived from gluten in gluten free bread and gluten free cracker. And we could detect peptides of 20 ppm wheat fortified to gluten free bread. We could detect other allergens shown on the label from commercial available food matrices.
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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.
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Improved R&D Efficiency Through Speedier Method Development (2)
An overview of this system was introduced in Technical Report vol. 33 “Improved R&D Efficiency Through Speedier Method Development (1).” In this report we introduce an example of the analytical method construction process for batch analysis of non-steroidal anti-inflammatory drugs.
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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.
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Characterization of Flavonoids and Phytoestrogens in an Extract of Pueraria Mirifica by UHPLC-MS-MS
Renewed interest in P. mirifica 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. This poster presents a selective and sensitive UHPLC-MS-MS method for meeting these requirements.
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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.
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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
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CLAM-2000 Application - Fully automated platform for determinatino of Benzodiazepines in serum
Fully Automated sample preparation procedure resulted suitable for the quantitation of Benzodiazepines by elimination of all manual preparation steps. The automation of the method increases the analytical performance, reduces the risk for human operators and due to the reduced reagent consumption, reduces also the cost of the analysis.
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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.
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GCMS Application - GC-MS Application for Artificial Photosynthesis Research (Japan)
Quantitation of hepcidin was tested using the LCMS 8050 triple quadruple mass spectrometer.
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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.
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High-Speed Analysis of Glycyrrhizinate
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High-Speed Analysis of Berberine
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High-Speed Analysis of Catechins
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High-Speed Analysis of Curcumin
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Full Automation with Integrated LC
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Selecting Detectors for Compounds with No Optical Absorbance
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Prominence nano System and Applications
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LCMS-8050 Application - A Rapid and Reproducible Immuno-MS Platform from Sample Collection to Quantitation of IgG (SSI)
This application news aims to provide a general model on using GC-MS to determine the amount of VOCs in water-based paints and varnishes, in anticipation of any emerging regulations in the near future. Referring to the method described in ISO 11890-2:2013, thirty-five commonly used solvents in water-based paints and varnishes are analyzed and quantified.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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LCMS-8060 Application - Development of Simplified Quantitative Method for Tryptic Digested C-reactive Protein by using Online SPE Coupled to Triple Quadrupole Mass Spectrometer (Japan)
Method development for accurate quantification of biomarker protein is very important step for the researchers in pharmaceutical industries and clinical fields. Mass spectrometry based quantitative proteomics approach shows a big potential to be the substitution of ELISA due to its precision, accuracy and multiplexing capability. In order to achieve the required sensitivity and selectivity, nano scale liquid chromatography mass spectrometry or sample preparation method including depletion of dominant protein and/or enrichment of target protein are frequently used. In this study, we tried to develop simple and high sensitive quantification method for C reactive protein (CRP), the level of which rise as a result of in ammation etc., by using online SPE coupled to triple quadrupole mass spectrometer without any complicated sample enrichment and depletion.
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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.
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LCMS-8060 Application - Quantitative Multi Target Screen (MTS) using liquid chromatography-tandem mass spectrometry with MS/MS library based identification for forensic toxicology
Multi Target Screening (MTS) has been applied to systemic toxicological analysis to reduce false positive and negative reporting using MS/MS spectral library based identi cation. MTS methods uses threshold triggered multiple reaction monitoring (MRM) and MS/MS product ion scans at three collision energies to confirm the compound identification based on mass spectral library searching. The MS/MS library was created using certified reference materials and included electrospray spectral data from over 1200 compounds relevant to clinical and forensic toxicology in both positive and negative ion modes. The MTS approach was applied to screening whole blood samples at three concentration levels to evaluate screening at therapeutic, overdose and toxic concentrations.
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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.
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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.
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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.
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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.
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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.
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LCMS-8060 Application - High Sensitivity Analysis of Peanut Allergen in Cumin and Spice Mix (Japan)
Food allergens are a major public health concern. Among them, peanut allergy is one of the common food allergies. To avoid unexpected contact with food allergens, food labels are strictly used to indicate the presence of specific allergens. With the increasing awareness of food allergies, the presence of undeclared peanut in cumin lead to huge recalls in recent years. Although ELISA is the most commonly used technique to detect allergens, its false-positive rate is a major concern due to its cross-reactivity. We developed a method with high specificity and sensitivity to overcome this issue by using a high sensitivity triple quadrupole mass spectrometer to detect peanut allergen Ara h1 in commercially available spices and seasonings.
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Development of simpli#31;ed quantitative method for tryptic digested C-reactive protein by using online SPE coupled to triple quadrupole mass spectrometer
Method development for accurate quanti#31;cation of biomarker protein is very important step for the researchers in pharmaceutical industries and clinical #31;elds. Mass spectrometry based quantitative proteomics approach shows a big potential to be the substitution of ELISA due to its precision, accuracy and multiplexing capability. In order to achieve the required sensitivity and selectivity, nano scale liquid chromatography mass spectrometry or sample preparation method including depletion of dominant protein and/or enrichment of target protein are frequently used. In this study, we tried to develop simple and high sensitive quanti#31;cation method for C reactive protein (CRP), the level of which rise as a result of in#30;ammation etc., by using online SPE coupled to triple quadrupole mass spectrometer without any complicated sample enrichment and depletion.
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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.
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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.
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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).
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LCMS-8060 Application - Applying 'MRM Spectrum Mode' and Library Searching for Enhanced Reporting Confidence in Routine Pesticide Residue Analysis (UK)
To help reduce the incidence of false positive and false negative reporting in pesticide residue monitoring routine multiple-reaction monitoring (MRM) methods have been enhanced to monitor a higher number of fragment ion transitions to increase specificity and reporting confidence. In this workflow, typically 6-10 fragment ion transitions were monitored for each target pesticide as opposed to a conventional approach using 2-3 fragment ions. By acquiring a high number of fragment ion transitions, each target pesticide had a corresponding fragmentation spectra which could be used in routine library searching and compound verification using reference library match scores. This ‘MRM Spectrum Mode’ was applied to quantify and identify 193 pesticides using 1,291 MRM transitions without compromising limits of detection, linearity or repeatability.
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LCMS-8060 Application - MRM based phospholipid profiling of mouse tissues by an ultra-fast triple quadrupole mass spectrometer
Phospholipids (PLs) serve as cell membrane structure holding various fatty acids such as arachidonic acid (AA) or docosahexaenoic acid (DHA). Although multiple reaction monitoring (MRM) using triple quadrupole mass spectrometer (TQ-MS) is expected to be the better sensitivity than scan or Q-TOF based method, theoretical number of PLs reaches several thousands, which is hard to be covered by MRM based method. Hence we have narrowed down the target PLs to develop over 400 polar head monitoring MRM and over 800 MRM for fatty acid determination using an ultra-fast TQ-MS. The MRM based method is expected to be better for finding out the minor PLs. Here we report PLs profiling results of mouse tissues using the MRM based method.
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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.
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LCMS-8060 Application - Toxicological screening for over 1000 compounds in a MRM based acquisition for Library ID in whole blood samples
A library of product ion spectra for 1222 compounds has been developed for clinical and forensic toxicology screening to help reduce false positive and false negative reporting. The library enables multi-targeted methods to be developed for routine screening, library identification and quantitation. The scope of the library considers two approaches; a MRM triggered full scan product ion spectra and MRM Spectrum mode. MRM Spectrum mode acquires a high number of fragment ion transitions for each target compound generating a fragmentation spectra which can be used in routine library searching and compound verification using reference library match scores. Both approaches have been applied to toxicological screening in a routine clinical laboratory using a triple quadrupole MS/MS platform.
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LCMS-8060 Application - Quantitative clinical toxicological screening comparing Library ID from product ion scane MS/MS to MRM Spectrum mode
Forensic toxicological sample measurement is commonly performed in a targeted analysis on selected panels of compounds. When using triple quadrupole platforms for analysis, typically two MRMs are used for compound measurement with a quantifier ion transition and reference ion transition. To help reduce false positive and false negative reporting two alternative approaches have been considered; MRM triggered product ion spectrum and MRM Spectrum mode. 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. In this work, we compare different approaches in target quantitation and identification applied to clinical and forensic toxicology
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LCMS-8060 Application - Applying 'MRM Spectrum Mode' and Library Searching for Enhanced Reporting Confidence in Routine Pesticide Residue Analysis
To help reduce the incidence of false positive and false negative reporting in pesticide residue monitoring routine multiple-reaction monitoring (MRM) methods have been enhanced to monitor a higher number of fragment ion transitions to increase specificity and reporting confidence. In this workflow, typically 6-10 fragment ion transitions were monitored for each target pesticide as opposed to a conventional approach using 2-3 fragment ions. By acquiring a high number of fragment ion transitions, each target pesticide had a corresponding fragmentation spectra which could be used in routine library searching and compound verification using reference library match scores. This 'MRM Spectrum mode' was applied to quantify and identify 193 pesticides using 1,291 MRM transitions without compromising limits of detection, linearity or repeatability using a high speed data acquisition triple quadrupole MS/MS.
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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.
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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.
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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.
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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.
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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.
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GC Application - Analysis of Epichlorohydrin Dissolved from Metal Food Cans by GC
Here we introduce an example of the separation and qualitative analysis of impurities in the widely used dye, Ru N719, using the LCMS-2020.
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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.
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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.
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GCMS-QP2010 Ultra Application - Determination of Fatty-acid Composition of Lipids in Human Embryonic Stem Cells Using GC-MS (Japan)
Using LCMS-8040, simultaneous detection method of eicosanoids and PAF was developed. 54 MRM transitions for 50 eicosanoids and PAF (platelet activation factor) were optimized. Limit of quantitation for several targets was in the subpicogram range.
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TOC Application - TOC - TOC Application Handbook Version 2
Quantification of testosterone in serum using an internal standard calibration on a LCMS-8050 triple quadrupole mass spectrometer was performed. Two MRM transitions for testosterone were monitored and the limit of detection in serum was in the femtograms (fg) level on column.
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GCMS-QP2010 SE Application - Introduction to Environmental Testing in the USA
In this method, we favour GCMS for its orthogonality to LCMS, peak capacity, inlet selectivity and the informing power of full scan spectra. We also wish to exploit GCMSMS for the detection and possible quantitation of target compounds. We believe that the use of simultaneous scan for non-targeted screening and MRM for targeted analysis has the potential to improve workflow and also support profiling and unknown detection in the analysis of urine specimens.
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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.
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TOC Application - TOC-L - Measurement of TOC and TN in Marine Water Algae Culture Solution
Seventy six analytes and their internal standards are described below. Multiple drug classes (barbituates, opiates, amphetamines, tricyclic antidepressants, synthetic cannabinoids, cannabinoids, club drugs, bath salts and hypnotics) were analyzed in a five minute polarity switching LCMS-8050 method.
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Using Headspace SPME-GC×GC–quadMS for the Characterization of Marsala Wine (Japan)
Plasma is an important matrix to measure the exposure of the drug prior to elimination. Clinical research often requires that drug concentrations in blood be monitored. The capability of the LCMS-8050 to detect low concentrations of drugs in plasma was evaluated.
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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
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High-Speed Analysis of Chlorogenic Acid
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High-Speed Analysis of Artificial Colorant
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High-Speed Drug Analysis
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Analysis of Dietary Supplements
Analytical Instrumentation & Software for the Evaluation, Identification and QA/QC of Dietary Supplements
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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.
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Structural Elucidation by Composition Formula Predictor Software Using MSn Data
Discerning the chemical formula or structure of unknowns is a difficult task which can be partially alleviated by acquiring high mass accuracy data; however, data interpretation is tedious and time consuming. By using fragmentation spectra collected from a novel hybrid ion-trap time-of-flight (IT-TOF) mass spectrometer along with enhanced software, samples are rapidly analyzed to identify chemical formulas and structures.
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Isotope modeling routines applied to empirical formula prediction
High mass accuracy mass spectrometry is achievable on a number of technology platforms including time of flight mass analyzers, hybrid ion trap and quadrupole time TOF&acute;s to FT-MS. Such technologies are playing an increasing role in pharmaceutical drug characterization and metabolite identification to help identify or confirm empirical formulae assignments. Recently, software tools have been applied to modeling theoretical isotopic distributions and mass accuracy data with experimentally derived data together with sets of chemical or statistical rules to help increase the probability of assigning the correct empirical formula.
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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>
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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LCMS-8060 Application - Full automated online sample extraction and analysis of mycotoxins in foods by online SFE-SFC-MS
Mycotoxins are low-molecular-weight natural products produced by fungi and are capable of causing disease and death. They are strictly regulated around the world because of their strong carcinogenic effects. A simple and reliable method to analyze mycotoxins is required to ensure food safety. The current methods require time-consuming sample pretreatment. Here we report a fully automated online sample extraction and analysis of mycotoxins in foods by online SFE-SFC-MS.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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Analysis of butylene glycol oligomer samples by temperature-rising direct analysis in real time mass spectrometry (TR-DART-MS)
DART (Direct Analysis in Real Time), a direct atmospheric pressure ionization source, is capable of analyzing chemical materials with little or no sample preparation. In DART analysis, as samples are only introduced into the heated helium gas #31;ow which is set at the preset temperature, they can be analyzed in a quite short time such as about 10 seconds. We had developed the temperature rising device, ionRocket, combined with DART-MS system (TR-DART-MS), which could make the heating temperature of sample rise with the passage of time. It became able to acquire a MS spectrum while changing the heating temperature successively by this. Here, we report the analyses of 1,3-butylene glycol oligomer samples using this temperature rising device.
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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.
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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.
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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.
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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.
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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.
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LCMS-8060 Application - High sensitive analysis of peanut allergen in cumin and spice mix
Food allergens are a major public health concern. Among them, peanut allergy is one of the common food allergies. To avoid unexpected contact with food allergens, food labels are strictly used to indicate the presence of speci#31;c allergens. With the increasing awareness of food allergies, the presence of undeclared peanut in cumin lead to huge recalls in recent years. Although ELISA is one of commonly used technique to detect allergens, its false-positive rate is a major concern due to its cross-reactivity. We developed a method with high speci#31;city and sensitivity to overcome this issue by using a high sensitivity triple quadrupole mass spectrometer to detect peanut allergen Ara h1 (Figure 1) in commercially available spices and seasonings.
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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).
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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.
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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.
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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.
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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.
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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).
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UV-Vis Application - UV Talk Letter - (1) Instrument Validation and Inspection Methods (2) Introduction to Sippers that are Effective for Muyltisample Continuous Measurements V8 C101-E122
Sensitivity was tested for four steroids on the LCMS- 8030 triple quadrupole mass spectrometer coupled with a Nexera UHPLC.
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GCMS-QP2010 Ultra Application - Sugar and Sterol Analysis in Human Body Fluids on a True Dual Column GCMS System (Japan)
In this Technical Report, we used the LCMS-8030 triple quadrupole mass spectrometer to evaluate whether or not 10 pesticide compounds used to spike a matrix at 10 ppb each could be detected automatically by using generic peak detection method in the screening for 176 pesticides using 1 msec pause and 5 msec dwell times.
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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.
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GCMS-QP2010 Ultra Application - Analysis of Pefume Allergens by using Comprehensive 2D GC and a Rapid-Scanning Quadrupole Mass Spectrometer (Japan)
Quantification of human IgG using an automated online trypsin digestion platform coupled directly to LCMS-8050 triple quadrupole mass spectrometer was performed. Two common peptides for IgG were monitored and the limits of detection were in the low fmol levels on column.
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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.
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GCMS-TQ8030 Application - Analysis of Pesticides in Citrus Oil Using a Shimadzu GCMS-TQ8030 (SSI)
Here, we have developed an online-SPE method to considerably shorten the pre-treatment time. In addition to optimisation of the extraction method, chromatographic separation was optimised to decrease ion-suppression and isobaric interference. Compound ionisation was enhanced using a new heated ESI (HESI) source on the LCMS-8050 triple quadrupole mass spectrometer.
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GCMS-TQ8040 Application - Drugs in Urine by GC-MS/MS Scan/MRM (SOPS)
Energy production is essential for every living organism. Energy production at the cellular level is carried out by various metabolic processes, including the glycolytic system and the TCA cycle. In order to investigate the metabolism of living systems, it is important to quantify the amount of each metabolite. However, many primary metabolites are hydrophilic and difficult to analyze by reversedphase chromatography. Ion pair chromatography is sometimes used for the analysis of such hydrophilic compounds but it is not preferable for LCMS analysis because ion pair reagents cause high background signals and sensitivity deterioration.
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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.
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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.
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GCMS-TQ8040 Application - Simultaneous Analysis of 477 Residual Pesticides in Agricultural Crops Using GC-MS/MS - Part 1 (Japan)
Anti-cancer research requires large volumes of samples covering a wide range of drugs to be analyzed. This can strain laboratory resources and impede the generation of analytical data necessary to accomplish research goals. The LCMS-8050 triple quadrupole mass spectrometer which combines industry leading UHPLC, scanning speeds, and detection limits was evaluated.
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GC Application - Trace Impurity Anlaysis of Hydrogen Fuel in Fuel Cell Vehicle-Related Fields
Recent developments in triple quadrupole mass spectrometry have delivered higher sensitivity, lower detection limits and faster data acquisition speeds generating enhanced data quality. To further improve peak area response and higher sensitivity, the ion sampling efficiency, transmission and detection on a high-end triple quadrupole MS/MS system LCMS-8050 was modified whilst still supporting a fast polarity switching time of 5 ms and data acquisition speeds of 30,000 u/sec.
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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.
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Fast and sensitive analysis of drug residues in water using on line SPE-UHPLC-MS/MS with ultra-fast polarity switching
As monitoring of drug residue in drinking and surface water is becoming of major concern in western countries, the environmental laboratories must face the increase in analysis request as well as the increase in the number of compounds to be screened. In parallel, as long as no consensus as been found on regulatory reporting levels, the assay sensitivity must be very high to not miss any compound. Thus, laboratories need a simple, rapid, reliable, sensitive and cost effective method to screen and to accurately quantify drug residues in a variety of water samples. A method was then set up to ful#31;ll these requirements. On line SPE is a useful tool to enable large sample volume injections. But due to the chemical diversity of target compounds, sample clean up cannot be pushed too far to not lose polar compounds. Then matrix effect or ion suppression can be problematic for accurate quanti#31;cation. Then, a very sensitive Mass Spectrometer as well as very effi#31;cient chromatography were necessary to compensate the relatively low sample volume injection. An innovative SPE set up was developed to combine low pressure on line SPE and high pressure UHPLC analysis.
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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.
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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.
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MSn analysis Identification of Molecular Species of Phospholipids by combination of Neutral Loss Survey and MS3
To elucidate the function of phospholipids, it is necessary to analyze not only their classes and subclasses but also molecular species. Recently, in the analysis of phospholipids, the application of mass spectrometry (MS) has become increasingly popular.
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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.
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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.
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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.
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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.
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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.
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Precise Identification of Molecular Species of Phosphatidylethanolamine and Phosphatidylserine by Neutral Loss Survey with MS3 and Accurate Mass Measurement
To elucidate the function of phospholipids, it is important to analyze not only their classes and subclasses but also molecular species. We found that electrospray ionization (ESI) MS3 analysis is effective for more detailed and accurate annotation of each molecular species. We established the system for analyses of molecular species of phospholipids with neutral loss (NL) survey of the head group-relating mass values and succeeding MS3 analyses by selecting the resulting product ions as precursor ions for MS3 analyses (Fig.1).
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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.
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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.
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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.
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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.
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Multi-residue analysis of pesticides in agricultural products using QuEChERS and SFC/MS
Analysis of pesticide residues in food is typically time-consuming due to the separation for multiple pesticides with a wide range of polarity and matrix co-eluting issues. To deal with the ever-growing number of pesticides, food safety laboratories need to ideally screen as many compounds as possible in a short time which may exceed maximum residual limits; typically 10 ppb in food matrices. Supercritical #31;uid chromatography (SFC) is one of the separation techniques, and it offers high resolution at high #31;ow rates and various separation modes. Therefore, it has the potential to separate multiple pesticides in a single run. In this study, we developed an analytical method for 441 pesticides in food matrices by QuEChERS and SFC/MS.
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Fully automated online sample extraction and analysis of mycotoxins in foods by online SFE-SFC-MS
Mycotoxins are low-molecular-weight natural products produced by fungi and are capable of causing disease and death. They are strictly regulated around the world because of their strong carcinogenic effects. A simple and reliable method to analyze mycotoxins is required to ensure food safety. The current methods require time-consuming sample pretreatment. Here we report a fully automated online sample extraction and analysis of mycotoxins in foods by online SFE-SFC-MS.
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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.
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Development of Automated Screening and Quantitation Approach on Novel On-Line SFE-SFC-MS/MS Platform – (I) For 23 Restricted Per#31;urocompounds in Textiles
Supercritical Fluid Chromatography (SFC) with carbon dioxide as eluent has attracted attention recently because of its advantages in low running cost, non-toxicity and wider coverage of analytes in terms of polarity. The combination of SFC with SFE (E=Extraction) has extended the applications to fully-automated sample pre-treatment and analysis as demonstrated by the Nexera UC system introduced by Shimadzu recently. The novel SFE-SFC-MS/MS system has been used successfully for analysis of 510 residual pesticides in agricultural products. One of the main advantages of the Nexera UC platform allows to set up on-line method to analyse directly different types and forms of un-pretreated samples. We describe the development of an approach on the Nexera UC platform, aiming at screening and quantitation of 23 per#31;urocompounds (PFCs) listed under the Restricted Substance List (RSL) in textile, leather and consumer goods industries.
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Quantitative Multi Target Screen (MTS) using liquid chromatography-tandem mass spectrometry with MS/MS library based identification for forensic toxicology
Multi Target Screening (MTS) has been applied to systemic toxicological analysis to reduce false positive and negative reporting using MS/MS spectral library based identi#31;cation. MTS methods uses threshold triggered multiple reaction monitoring (MRM) and MS/MS product ion scans at three collision energies to con#31;rm the compound identi#31;cation based on mass spectral library searching. The MS/MS library was created using certi#31;ed reference materials and included electrospray spectral data from over 1200 compounds relevant to clinical and forensic toxicology in both positive and negative ion modes. The MTS approach was applied to screening whole blood samples at three concentration levels to evaluate screening at therapeutic, overdose and toxic concentrations.
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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
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Development of Automated Screening and Quantitation Approach on Novel On-Line SFE-SFC-MS/MS Platform- (II) for FIve Aflatoxins in Powdered Food Samples
Supercritical #31;uid chromatography (SFC) is one of the trendy analytical techniques in recent years. By using carbon dioxide (CO2) as eluent, the SFC has a number of advantages like environmental friendly, cost effective and suitable for a wide range of analytes’ polarities. The Nexera UC system (Shimadzu) is a further developed platform combining SFE (extraction) and SFC with MS/MS into a complete system to handle from sample pre-treatment and separation to superior MS/MS detection and quantitation in a fully automated manner. The novel SFE-SFC-MS/MS system has been used successfully for analysis of 510 residual pesticides in agricultural products [1]. Here we describe the applications and advantages of the Nexera UC system in analysis of afl#31;atoxins (B1, B2, G1, G2 and M1) in powdered food such as corn #31;our and wheat fl#31;our.
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Pesticide analysis in complex food extracts by multi-transition MRM and library searching for enhanced residue con#31;rmation
In this work, a conventional MRM method developed for routine pesticide analysis (typically monitoring 2-3 MRM transitions for each pesticide) has been modi#31;ed and extended to include a higher number of MRM transitions speci#31;c to each pesticide compound (dependent on the pesticide in question, typically 6-12 fragment ions per-compound are monitored). This approach has not been possible on previous MS instruments due to the limited duty cycle resulting in shorter dwell times or an increased cycle time for each MRM and as a consequence lower peak sampling rates and lower sensitivity. Using a fast scanning triple quadrupole mass spectrometer this approach was applied to the routine analysis of a panel of 202 pesticides spiked into a matrix.
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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.
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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.
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