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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Aqueous extraction followed by derivatization and liquid chromatography-mass spectrometry analysis: A unique strategy for trace detection and identification of G-nerve agents in environmental matrices
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Aqueous extraction followed by derivatization and liquid chromatography-mass spectrometry analysis: A unique strategy for trace detection and identification of G-nerve agents in environmental matrices

机译:水性提取,然后进行衍生化和液相色谱 - 质谱分析:痕量检测和鉴定环境基质中G-T神经试剂的独特策略

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A highly sensitive method for the detection and identification of sarin (GB), soman (GD) and cyclosarin (GF) chemical warfare agents (CWAs) in environmental outdoor and indoor matrices such as soil, asphalt, linoleum, formica, concrete and cloth was developed. The method incorporates derivatization of the G-type nerve agent extracts with 2-Rdimethylamino)methyllphenol (2-DMAMP), followed by LC-ESI(+)-MS/MS analysis. Four LC-amenable extraction solvents were explored in terms of their extraction efficiency and the reaction rate of the derivatizing agent. The reaction time, temperature and derivatization reagent amount were optimized. The optimal procedure was found to be extraction with water by agitation (2 min), followed by the addition of 2-DMAMP directly into the injection vial and stirring for 5 min prior to LC-ESI(+)-MS/MS analysis, without any other pretreatment. The method was applied to real-world samples and exhibited very low detection limits (LODs) of 0.8-20 pg/cm(2) in asphalt, linoleum, cloth, formica and concrete and 4 pg/g in soil. The newly developed method demonstrated significantly superior sensitivity compared to conventional GC-MS- and LC-MS-based methods for the identification of G-nerve agents and allowed the determination of both G-nerve agents and their hydrolysis products within a single LC-MS/MS run. The proposed methodology may be practical for verifying contaminated matrices collected in the battlefield or terror scenes in forensic investigations where trace level analysis is required. (C) 2018 Elsevier B.V. All rights reserved.
机译:在环境室外和室外基质中检测和鉴定Sarin(GB),Soman(Gd)和环己烷(GF)的高度敏感方法,如土壤,沥青,油毡,晶体,混凝土和布料发达。该方法包括与2- rdimethylamino)甲基苯酚(2-Dmamp)的G型神经试剂提取物的衍生化,其次是LC-ESI(+) - MS / MS分析。在其提取效率和衍生剂的反应速率方面探讨了四种LC允许的萃取溶剂。优化反应时间,温度和衍生化试剂量。发现最佳过程用搅拌(2分钟)用水萃取,然后将2-Dmamp直接加入注射小瓶中,并在LC-ESI(+) - MS / MS分析之前搅拌5分钟,没有任何其他预处理。将该方法应用于现实世界上的样品,并在沥青,油毡,布,晶状体和混凝土中表现出0.8-20pg / cm(2)的非常低的检测限率(LOD),以及土壤中的4 pg / g。与常规GC-MS和LC-MS的方法相比,新开发的方法对鉴定G-神经剂的方法进行了显着优异的敏感性,并允许在单个LC-MS内测定G-T神经试剂及其水解产物/ MS运行。所提出的方法可能是实用的,用于验证在需要进行痕量水平分析的法医调查中收集的战场或恐怖场景中收集的受污染矩阵。 (c)2018年elestvier b.v.保留所有权利。

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