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Optimisation and validation of a GC-MS/MS method for the analysis of methyl salicylate in hair and skin samples for use in human-volunteer decontamination studies

TitleOptimisation and validation of a GC-MS/MS method for the analysis of methyl salicylate in hair and skin samples for use in human-volunteer decontamination studies
Publication TypeJournal Article
Year of Publication2019
AuthorsJames T., Collins S., Amlot R., Marczylo T.
JournalJ Chromatogr B Analyt Technol Biomed Life Sci
Volume1109
Pagination84-89
Date PublishedMar 1
ISBN Number1570-0232 (Linking)
Accession Number30738341
KeywordsCalibration, DECONTAMINATION, Decontamination/*methods, Gas Chromatography-Mass Spectrometry/*methods/standards, Gc-ms/ms, Hair/*chemistry, Human samples, Humans, Limit of Detection, Linear Models, methyl salicylate, Optimisation, Reproducibility of Results, Salicylates/*analysis, simulant, Skin/*chemistry
Abstract

Methyl salicylate has a long history of use as a chemical warfare agent simulant for volatile lipophilic compounds such as sulphur mustard. An improved isotope dilution GC-MS/MS method was developed, optimised and validated for the analysis of methyl salicylate in human skin and hair samples, for use in emergency decontamination volunteer studies. Following derivatisation, quantification was measured on a triple quadrupole mass spectrometer, set to EI mode and conducting multiple reaction monitoring of target ions. The mass transitions were 209-->179 and 213-->161 for quantitation of methyl salicylate and methyl salicylate D4, respectively whereas qualifier ion transitions used to verify identity were 209-->169 and 213-->89. The method achieved excellent coefficient of determination (R(2)>0.9968 to 0.9999) over the range of 0.5-5000ng/ml and the LOD and LOQ were 0.05ng/ml and 0.5ng/ml. The method was further validated for accuracy (intra-day and inter-day average 100.28% to 102.03% and 99.48% to 102.33%, respectively) and precision (intra-day RSD 1.43% to 2.35%, inter-day RSD 1.91% to 2.97%) at three concentrations (25, 250 and 2500ng/ml). The validated method was successfully used to identify methyl salicylate in samples of human skin generated during volunteer studies of emergency decontamination systems and in hair of staff conducting these studies.

URLhttps://www.ncbi.nlm.nih.gov/pubmed/30738341
DOI10.1016/j.jchromb.2019.01.030
Short TitleOptimisation and validation of a GC-MS/MS method for the analysis of methyl salicylate in hair and skin samples for use in human-volunteer decontamination studies

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