The Swedish Defence Research Agency, FOI CBRN Defence and Security, SE-901 82 Umeå, Sweden.
Anal Chem. 2010 Sep 1;82(17):7452-9. doi: 10.1021/ac101604n.
A rapid screening and identification method based on derivatization and gas chromatography mass spectrometry (GC-MS) has been developed for the detection of alkylphosphonic acids (APAs), the degradation products of organophosphorus nerve agents. The novel method described involves rapid (5 min) and direct derivatization of 25 microL aqueous sample using highly fluorinated phenyldiazomethane reagents (e.g., 1-(diazomethyl)-3,5-bis(trifluoromethyl)benzene). The APA derivatives are then screened by GC-MS negative ion chemical ionization (NICI) and identified by electron ionization (EI) mode. The conditions for the derivatization were optimized using statistical experimental design and multivariate data analysis. Method robustness was evaluated using aqueous samples from an official OPCW Proficiency Test and all APAs present in the sample were conclusively identified. Limits of detection for rapid screening using SIM NICI were between 5 and 10 ng/mL APA in aqueous sample, and for identification using full scan EI 100 ng/mL.
已开发出一种基于衍生化和气相色谱质谱联用（GC-MS）的快速筛选和鉴定方法，用于检测烷基膦酸（APAs），这是有机磷神经毒剂的降解产物。所描述的新方法涉及使用高度氟化的苯重氮甲烷试剂（例如 1-（重氮甲基）-3,5-双（三氟甲基）苯）对 25 μL 水相样品进行快速（5 分钟）和直接衍生化。然后通过 GC-MS 负离子化学电离（NICI）筛选 APA 衍生物，并通过电子电离（EI）模式进行鉴定。通过统计实验设计和多元数据分析对衍生化条件进行了优化。使用来自官方 OPWC 能力验证的水样评估了方法的稳健性，并且对样品中存在的所有 APA 都进行了明确鉴定。使用 SIM NICI 进行快速筛选的检测限在 5 到 10 ng/mL APA 之间，而使用全扫描 EI 进行鉴定的检测限为 100 ng/mL。
