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Direct derivatization and gas chromatography-tandem mass spectrometry identification of nerve agent biomarkers in urine samples
Umeå University, Faculty of Science and Technology, Department of Chemistry.
2013 (English)In: Journal of chromatography. B, ISSN 1570-0232, E-ISSN 1873-376X, Vol. 928, 98-105 p.Article in journal (Refereed) Published
Abstract [en]

Rapid determination of nerve agent biomarkers at low-ppb levels in urine samples was achieved by direct derivatization and sample analysis using gas chromatography-tandem mass spectrometry. The studied biomarkers were alkylphosphonic acids (APAs), as they are specific hydrolysis products of organophosphorus nerve agents that can be used to verify nerve agent exposure. The sample preparation technique employed involves rapid direct derivatization (5min) of acidified urine samples (25μL) using a highly fluorinated phenyldiazomethane reagent [1-(diazomethyl)-3,5-bis(trifluoromethyl)benzene]. The derivatization conditions were optimized using statistical experimental design and multivariate data analysis. The APA derivatives were analyzed by GC-MS and MS/MS using negative ion chemical ionization. The selectivity and sensitivity of analyses performed by low and high resolution single ion monitoring MS-mode were compared with those performed by multiple reaction monitoring MS/MS-mode. The MS/MS technique offered the greatest sensitivity and selectivity of the tested mass spectrometric techniques, with limits of detection ranging from 0.5 to 1ng APAs/mL of urine. The method's robustness was evaluated using urine samples from the OPCW 2nd biomedical confidence building exercise and all APAs present in the samples were conclusively identified. The method thus offers excellent performance and is viable for the simultaneous trace determination of a wide range of nerve agent markers.

Place, publisher, year, edition, pages
Elsevier, 2013. Vol. 928, 98-105 p.
Keyword [en]
Chemical warfare agents, Organophosphorus nerve agents, Alkylphosphonic acids, Biomedical samples, Direct derivatization
National Category
Analytical Chemistry
URN: urn:nbn:se:umu:diva-73124DOI: 10.1016/j.jchromb.2013.03.009ISI: 000319236700013PubMedID: 23603296OAI: diva2:630459
Available from: 2013-06-19 Created: 2013-06-17 Last updated: 2013-07-02Bibliographically approved

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Subramaniam, Raja
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