气相色谱负离子化学电离质谱测定环境中土壤与水中硫丹及其代谢物

Determination of Endosulfans and its Metabolite in the Soil and Water Samples by Gas Chromatography-Mass Spectrometry with Negative Ionization Mode

建立一种气相色谱负离子化学电离质谱(GC-NCI-MS)测定环境中土壤和水中硫丹及其代谢物残留的检测方法,环境中土壤样用丙酮/水浸渍,乙酸乙酯提取,固相萃取小柱净化,水样经乙酸乙酯提取,采用GC-NCI-MS选择离子监测方式进行定性和定量分析,以外标法定量,方法中每种化合物的检出限土壤为0.05μg/kg,水为0.005μg/L,在方法的检测限与50μg/kg(5μg/L)范围内,线性相关系数大于0.999 5,在所添加三个浓度水平下,方法的回收率70%～95%,相对标准偏差(RSD)1.2%～11.8%。结果表明,该方法简便、快速、灵敏、精密度好,适合对环境中土壤和水样中硫丹及其代谢物进行有效监测。

A rapid and sensitive method based on GC-NCI-MS was established to detect the endosulfan and its metabolite in the soil and water samples.Prior to the qualitative and quantitative analysis fulfilled by GC-NCI-SIM,the soil samples were immersed by water/acetone,extracted by ethyl acetate and purified by SPE column whereas the water ones were directly extracted by ethyl acetate.In the soil and water samples,each compound has the limits of detection of 0.05 μg/kg and 0.005 μg/L respectively,with linear correlation coefficient of 0.999 5.The average recoveries from spiked samples at the three different concentrations ranged from 70%-95%,with relative standards deviation（RSD） of 1.2%-11.8%.The experimental results show that the developed methods is simple,rapid,sensitive and repetitive and may be effectively applied to the monitoring of endosulfans and its metabolite in the soil and water samples.