气相色谱-质谱法分析水和土壤中化学毒剂模拟剂

为了快速处理化学毒剂的突发性事故，建立了水和土壤中4种化学毒剂模拟剂的气相色谱 质谱（GC/MS）快速分析检测方法。水样用二氯甲烷和乙腈分两步进行萃取，土壤样品用二氯甲烷萃取，萃取液经HP 5MS色谱柱(30 m×0.25 mm×0.25 μm)分离，利用GC/MS的选择离子(SIM)模式进行定性和定量检测。结果表明：本方法可对水和土壤样品中的化学毒剂模拟剂进行分析，在0.1～10 mg/L质量浓度范围内，线性关系良好，相关系数为0.998 4～0.999 9。4种化合物在水中的检出限为0.3～2.1 μg/L，定量限为1.1～7.1 μg/L；在土壤中的检出限为1.0～2.7 μg/kg，定量限为3.4～8.8 μg/kg；4种化学毒剂模拟剂在水和土壤中的相对标准偏差(RSD)分别小于11.5%、11.8%；水和土壤中高、中、低3个加标水平的回收率分别为70.5%～101.9%、70.8%～112.9%。该方法快速准确、背景干扰少、分析灵敏度较高，适用于水和土壤样品中化学毒剂的快速分析。

GC/MS Analysis of Chemical Agent Simulants in Water and Soil

In order to rapid deal with the unexpected incidents of chemical agents,a method based on gas chromatography spectrometry(GC/MS) was developed for the determination of nerve warfare agent and vesicant agent simulants in water and soil.The water was extracted by dichloromethane and acetonitrile,the soil was extracted by dichloromethane,then the extract was separated on a HP-5MS column(30 m×0.25 mm×0.25 μm) and the identification and quantification of the analytes were carried out in the choice ion(SIM) mode.The six point calibration curves showed a good linearity for all the congeners(0.998 4~0.999 9).Limits of detection(LODs) of the water ranged from 0.3 to 2.1 μg/L and the soil ranged from 1.0 to 2.7 μg/kg.The relative standard deviations(RSDs) of water and soil were below 11.5%、11.8% respectively.The spiked recoveries of water and soil were in the range of 70.5%~101.9%、70.8%~112.9% respectively.The developed analytical method is rapid and accurate,remove the pigments effieient and improve sensitivity,suitable for the determination of warfare agents in water and soil.