土壤基质中4种典型化学毒剂的加速溶剂萃取-气相色谱法检测

Determination of Chemical Warfare Agents in Soil by Accelerated Solvent Extraction-Gas Chromatography

采用加速溶剂萃取法萃取土壤基质中的4种典型化学毒剂,萃取液用气相色谱-火焰光度检测器分析。当土壤中4种化学毒剂含量均为10 mg/kg时,用含5%三乙胺的二氯甲烷作萃取溶剂,在加压15 MPa,室温下提取7 min的条件下,沙林、梭曼、维埃克斯的回收率均超过80%,芥子气为73%。方法对土壤中沙林、梭曼和维埃克斯的检出限分别为1.8、1.4和70 ng/g(磷模式),对芥子气的检出限为500 ng/g(硫模式)。并与传统液-固萃取法进行了比较。

A rapid and effective method for determination of 4 chemical warfare agents（CWAs） in soil has been developed by using accelerated solvent extraction（ASE） -gas chromatography （GC） coupled with dual sulfur and phosphorous mode flame photometric detector （FPD-P/S）. Soil samples were extracted with ASE by using mixed solution oftriethylamine and dichloromethane （5 ： 95, by volume） as solvent and extraction pressure of 15 MPa at room temperature for 7 rain. Isopropyl methyl phosphonofluoridate （GB）, pinacolyl methylphosphonofluoridate（GD）, and O-ethyl S-2-diisopropylaminoethyl methylphosphonothioate （VX） were analyzed by GC with flame photometric detector in phosphorous mode, and dichloroethyl sulfide （HD） was analyzed in sulfur mode. The recoveries of CWAs from the spiked soil sample were range of 73% - 88%. The detection limits of GB, GD, VX and HD were 1.8, 1.4, 70 and 500 ng/g, respectively. The result obtained showed that this method was obviously better than the traditional liquid -solid extraction（LSE） method in the aspects of recoveries, sensitivity, consume solvent and consume time.