DOI: 10.3724/SP.J.1096.2013.30245

Chinese Journal of Analytical Chemistry (分析化学) 2013/41:12 PP.1801-1806

A New High Performance Liquid Chromatography Tandem Mass Spectrometric Method for Quantitative Determination of Soman-tyrosine Adduct in Exposed Rat Plasma

Towards the urgent need of accurately retrospective analysis of biomedical samples exposed by nerve agent soman (GD), we developed a new quantitative method of GD-tyrosine adduct (GD-Tyr) in exposed rat plasma by liquid chromatography (LC)-tandem mass spectrometry (MS/MS) with high sensitivity and high specificity. After a series of pretreatment procedures including extraction of albumin by affinity chromatography and ultrafiltration, enzymatic hydrolysis by pronase, and solid phase extraction, we qualitatively and quantitatively determined soman-tyrosine adduct by reversed-phase LC-triple quadrupole MS in the positive electrospray ionization and multiple reactions monitoring mode. The monitored transitions were m/z 260/214 (GD-Tyr) and m/z 293/247(internal standard). A good linearity was obtained in the range of 0.1-500 μg/L for GD-Tyr (R2=0.999) with a limit of detection of 0.02 μg/L and a limit of quantification of 0.05 μg/L. The recovery of GD-Tyr was in the range of 90.1%-103.5%, and the RSD of this method was less than 3%. We then investigated the toxicokinetics of GD-Tyr for GD exposed SD rat (n=5) in an intraperitoneal injection way. An obvious time and dose dependent relationship between GD-Tyr and the dose of soman was observed. We suggest that GD-tyrosine adduct can be used as an exposure biomarker to the retrospective detection of soman after exposure.

Key words:Soman,Soman-tyrosine adduct,Liquid chromatography-tandem mass spectrometry,Plasma,Toxicokinetics

ReleaseDate:2015-04-19 11:07:49

白海红, 郭 磊, 冯建林, 冯翠玲, 陈 佳, 谢剑炜. 分析化学, 2008, 36(9): 1269-1272

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