采用液相色谱-串联质谱法对饮料中化学战剂降解产物进行定量分析。
Quantitative analysis of chemical warfare agent degradation products in beverages by liquid chromatography tandem mass spectrometry.
机构信息
Forensic Science Center, Lawrence Livermore National Laboratory, L-091 Livermore, California 94550, USA.
出版信息
J Agric Food Chem. 2009 Sep 23;57(18):8227-35. doi: 10.1021/jf901478k.
Though chemical warfare agents (CWAs) have been banned by the Chemical Weapons Convention, the threat that such chemicals may be used, including their deliberate addition to food, remains. In such matrixes, CWAs may hydrolyze to phosphonic acids, which are good surrogate markers of CWA contamination. The method described here details the extraction of five CWA degradation products, including methylphosphonic acid (MPA), ethyl-MPA, isopropyl-MPA, cyclohexyl-MPA, and pinacolyl-MPA, from five different beverages by strata-X solid phase extraction cartridges. Samples were analyzed by liquid chromatography tandem mass spectrometry (LC/MS/MS) with multiple reaction monitoring. The limit of quantitation ranged from 0.05 to 0.5 ng on-column, and the limit of detection was >0.02 ng on-column. Beverages were fortified with the five phosphonic acids at 1 microg/mL and 0.25 microg/mL and quantitated using both an internally standardized method and matrix-matched standards. Reasonable recoveries (>50%) were achieved for ethyl, isopropyl, cyclohexyl, and pinacolyl-MPA for most matrixes.
尽管《化学武器公约》已经禁止了化学战剂（CWAs），但这些化学物质仍可能被用作武器，包括故意添加到食物中。在这些基质中，CWAs 可能会水解为膦酸，膦酸是 CWA 污染的良好替代标志物。本文介绍了一种从五种不同饮料中用 Strata-X 固相萃取小柱提取五种 CWA 降解产物（包括甲基膦酸（MPA）、乙基-MPA、异丙基-MPA、环己基-MPA 和频哪醇基-MPA）的方法。样品通过液相色谱串联质谱（LC/MS/MS）进行分析，采用多反应监测。在柱上的定量下限范围为 0.05 至 0.5ng，在柱上的检测限大于 0.02ng。在 1μg/mL 和 0.25μg/mL 时，用这五种膦酸对饮料进行强化，并使用内标法和基质匹配标准进行定量。对于大多数基质，乙基、异丙基、环己基和频哪醇基-MPA 的回收率均达到了 50%以上。
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