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Part 3: Solid Phase Extraction of Russian VX and its Chemical Attribution Signatures in Food Matrices and their Detection by GC-MS and LC-MS ☆
Talanta ( IF 5.6 ) Pub Date : 2018-03-17
Audrey M. Williams, Alexander K. Vu, Brian P. Mayer, Saphon Hok, Carlos A. Valdez, Armando Alcaraz

Chemical attribution signatures indicative of O-isobutyl S-(2-diethylaminoethyl) methylphosphonothioate (Russian VX) synthetic routes were investigated in spiked food samples. Attribution signatures were identified using a multifaceted approach: Russian VX was synthesized using six synthetic routes and the chemical attribution signatures identified by GC-MS and LC-MS. Three synthetic routes were then down selected and spiked into complex matrices: bottled water, baby food, milk, liquid eggs, and hot dogs. Sampling and extraction methodologies were developed for these materials and used to isolate the attribution signatures and Russian VX from each matrix. Recoveries greater than 60% were achieved for most signatures in all matrices; some signatures provided recoveries greater than 100%, indicating some degradation during sample preparation. A chemometric model was then developed and validated with the concatenated data from GC-MS and LC-MS analyses of the signatures; the classification results of the model were >75% for all samples. This work is part three of a three-part series in this issue of the United States-Sweden collaborative efforts towards the understanding of the chemical attribution signatures of Russian VX in crude materials and in food matrices.



中文翻译:

第3部分:食品基质中俄罗斯VX的固相萃取及其化学归属特征及其通过GC-MS和LC-MS的检测

表示O的化学属性签名对加标食品样品中的S-(2-二乙基氨基乙基)甲基硫代磷酸异丁酯(Russian VX)合成路线进行了研究。使用多方面的方法识别出特征标记:使用六种合成途径合成了俄罗斯VX,并通过GC-MS和LC-MS识别了化学特征标记。然后,从三种合成途径中选择了三种,并将它们掺入复杂的基质中:瓶装水,婴儿食品,牛奶,液态鸡蛋和热狗。针对这些材料开发了采样和提取方法,并用于从每个矩阵中分离出归因签名和俄罗斯VX。在所有基质中,大多数签名的回收率均超过60%;一些特征提供的回收率大于100%,表明样品制备过程中有些降解。然后开发了化学计量学模型,并使用来自GC-MS和LC-MS签名分析的关联数据进行了验证;所有样品的模型分类结果均> 75%。这项工作是本期美国与瑞典合作研究的三部分系列的第三部分,该系列文章旨在了解俄罗斯VX在原油原料和食品基质中的化学属性特征。

更新日期:2018-03-18
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