气相色谱-质谱法分析水和土壤中化学毒剂模拟剂

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

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(30m×0.25mm×0.25μm)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0.1～10mg/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0.3～2.1μg/L,定量限为1.1～7.1μg/L;在土壤中的检出限为1.0～2.7μg/kg,定量限为3.4～8.8μg/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。

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 ex- tracted by dichloromethane and aeetonitrile, the soil was extracted by dichloromethane,then the extract was separated on a HP-SMS 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 /,g/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 20,. 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.