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采用正相硅胶和超高效液相色谱-飞行时间质谱法(UPLC-TOF-MS)对食品中的沙林和 VX 进行痕量分析。

Trace Level Analysis of Sarin and VX in Food Using Normal Phase Silica Gel and Ultra-Performance Liquid Chromatography-Time-of-Flight Mass Spectrometry (UPLC-TOF-MS).

机构信息

Research and Technology Directorate , U.S. Army, Edgewood Chemical Biological Center (ECBC), Aberdeen Proving Ground , Maryland 21010-5424 , United States.

出版信息

J Agric Food Chem. 2018 Jul 25;66(29):7846-7856. doi: 10.1021/acs.jafc.8b01756. Epub 2018 Jul 11.

DOI:10.1021/acs.jafc.8b01756
PMID:29920090
Abstract

Ultra-Performance Liquid Chromatography/electrospray ionization mass spectrometry was used for the trace level determination of isopropyl methylphosphonofluoridate (Sarin, GB) and ( O-ethyl S-[2-(diisopropylamino)ethyl] methylphosphonothioate (VX) after extraction from various foods. A method utilizing normal phase silica gel was developed for the sample preparation and extraction of VX and GB from food. The extraction efficiencies of the normal phase silica gel method for VX was compared to those of other commercial solid phase extraction media and was found to be comparable. Sarin was found to be incompatible with both the mixed mode cation exchange (MCX) sorbents and QuEChERS methods that are commercially available but was successful with the normal phase silica gel method. The linear range of quantitation for VX was 0.1-330 ng/mL and for GB was 20-1200 ng/mL. The average recoveries of VX and GB from the various food matrices along with the corresponding relative standard deviations (RSDs) are reported.

摘要

超高效液相色谱/电喷雾电离质谱法用于痕量测定异丙基甲基膦酸氟化物(沙林,GB)和(O-乙基 S-[2-(二异丙基氨基)乙基]甲基膦酸硫酯(VX),从各种食品中提取。建立了一种利用正相硅胶的方法,用于从食品中提取 VX 和 GB。比较了正相硅胶法对 VX 的提取效率与其他商业固相萃取介质的提取效率,发现正相硅胶法相当。沙林与市售的混合模式阳离子交换(MCX)吸附剂和 QuEChERS 方法不兼容,但与正相硅胶法兼容。VX 的定量线性范围为 0.1-330ng/mL,GB 的定量线性范围为 20-1200ng/mL。报告了 VX 和 GB 从各种食品基质中的平均回收率以及相应的相对标准偏差(RSD)。

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