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填充毛细管液相色谱-电喷雾质谱法测定土壤中的沙林、梭曼及其水解产物。

Determination of sarin, soman and their hydrolysis products in soil by packed capillary liquid chromatography-electrospray mass spectrometry.

作者信息

D'Agostino P A, Hancock J R, Provost L R

机构信息

Defence Research Establishment Suffield, Medicine Hat, Alberta, Canada.

出版信息

J Chromatogr A. 2001 Apr 6;912(2):291-9. doi: 10.1016/s0021-9673(00)01275-9.

Abstract

An analytical method based on aqueous ultrasonic extraction and packed capillary liquid chromatography-electrospray mass spectrometry (LC-ESI-MS) analysis was developed and compared to an existing gas chromatography(GC)-MS based method for the determination of sarin, soman and their hydrolysis products in contaminated soil. Three soils, a red clay, a tan sandy clay and a brown sandy clay loam, were spiked with sarin and soman and their initial hydrolysis products, isopropyl methylphosphonic acid and pinacolyl methylphosphonic acid, at the 10 microg/g level to assess recovery efficiency. Recovery of sarin and soman from the aqueous soil extracts was comparable to the existing analytical method, with a significant improvement in recovery being demonstrated for the chemical warfare agent hydrolysis products. Sarin and soman were recovered in the 20-90% range from the three soil types with aqueous extraction, while the hydrolysis products of these chemical warfare agents were extracted with recoveries in excess of 80%. The developed soil extraction and analysis method appears to be an attractive alternative to the GC-MS based method, since aqueous extracts containing chemical warfare agent hydrolysis products may be analysed directly, eliminating the need for additional sample handling and derivatization steps.

摘要

开发了一种基于水相超声萃取和填充毛细管液相色谱 - 电喷雾质谱(LC - ESI - MS)分析的方法,并将其与现有的基于气相色谱(GC) - MS的方法进行比较,用于测定受污染土壤中的沙林、梭曼及其水解产物。三种土壤,即红粘土、棕褐色砂质粘土和棕色砂质粘壤土,分别以10微克/克的水平添加沙林、梭曼及其初始水解产物异丙基甲基膦酸和频哪基甲基膦酸,以评估回收率。从土壤水提取物中回收沙林和梭曼的情况与现有分析方法相当,化学战剂水解产物的回收率有显著提高。通过水相萃取,从三种土壤类型中回收沙林和梭曼的范围为20 - 90%,而这些化学战剂的水解产物的回收率超过80%。所开发的土壤萃取和分析方法似乎是基于GC - MS方法的一种有吸引力的替代方法,因为含有化学战剂水解产物的水提取物可以直接分析,无需额外的样品处理和衍生步骤。

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