Published: Journal of Analytical Toxicology, Volume 23, Number 2, March/April 1999, pp.86-93.
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 Miki1, Muneharo Katagi1, Hitoshi Tsuchihashi, and Masakazu Yamashita
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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