Journal Article

Determination of Alkylmethylphosphonic Acids, the Main Metabolites of Organophosphorus Nerve Agents, in Biofluids by Gas Chromatography-Mass Spectrometry and Liquid-Liquid-Solid-Phase-Transfer-Catalyzed Pentafluorobenzylation

Akihiro Miki, Muneharo Katagi, Hitoshi Tsuchihashi and Masakazu Yamashita

in Journal of Analytical Toxicology

Volume 23, issue 2, pages 86-93
Published in print March 1999 | ISSN: 0146-4760
Published online March 1999 | e-ISSN: 1945-2403 | DOI: http://dx.doi.org/10.1093/jat/23.2.86
Determination of Alkylmethylphosphonic Acids, the Main Metabolites of Organophosphorus Nerve Agents, in Biofluids by Gas Chromatography-Mass Spectrometry and Liquid-Liquid-Solid-Phase-Transfer-Catalyzed Pentafluorobenzylation

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A simple gas chromatography-mass spectrometry (GC-MS) procedure has been developed for the main metabolites of organophosphorus nerve agents, alkylmethylphosphonic acids (AMPAs; alkyl = Et, i-Pr, and pinacolyl) in biofluids via extractive pentafluorobenzylation. The derivatization was carried out under liquid-liquid-solid-phase-transfer conditions using a polymer-bound tri-n-butylmethylphosphonium bromide as a catalyst. AMPAs in aqueous samples were semiquantitatively extracted into a small-volume organic layer as their pentafluorobenzyl derivatives at pH 4.5 (85°C). Sample pretreatments for urine, serum, and saliva were each examined to minimize matrix interference. The detection limits of APMAs by electron-impact ionization GC-MS were around 50 ng/mL and 2.5–10 ng/mL in the full-scan and selected-ion monitoring modes, respectively. In order to detect trace-level AMPAs, negative-ion chemical ionization (NICI) was also employed to enhance sensitivity. The detection limits of AMPAs in biofluids were typically 60 pg/mL by GC-NICI-MS.

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Subjects: Medical Toxicology ; Toxicology (Non-medical)

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