LITERATURE


- 252 results found for "lcms"
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Perfluorocarbons
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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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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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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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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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-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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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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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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Accute poisoning with a rat bait
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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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Which column is your analysis based on?
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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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Natural Product Analysis using the LCMS-IT-TOF
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Opening LCMS to research: Psiport browser software
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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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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-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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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 - 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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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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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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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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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-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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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 - 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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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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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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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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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-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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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 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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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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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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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
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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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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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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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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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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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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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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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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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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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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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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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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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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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 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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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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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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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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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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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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Quantitative analysis of 646 pesticides (1,919 MRMs) by LC-MS/MS with a fast 10.5 minute cycle time.
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 speci#31;c 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#30;ows and support increased pesticide monitoring programs. Using the Shimadzu Pesticide MRM Library (the Library includes information on 766 certi#31;ed 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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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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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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