全自动在线顶空固相微萃取-气相色谱-串联质谱法测定鱼塘投毒案件水样中硫丹和硫丹硫酸酯  

GC-MS/MS Determination of Endosulfan and Endosulfan Sulfate in Fishpond Water Samples of Poisoning Cases with Fully Automatic Online HS-SPME

作　　者：王丹[1] 张云峰[2] 董林沛 姜红[1] WANG Dan;ZHANG Yunfeng;DONG Linpei;JIANG Hong(School of Investigation,People′s Public Security University of China,Beijing100038,China;Institute of Forensic Science Ministry of Public Security P.R.C.,Beijing100038,China)

机构地区：[1]中国人民公安大学侦查学院,北京100038 [2]公安部物证鉴定中心,北京100038

出　　处：《理化检验（化学分册）》2021年第2期108-113,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：中央级公益性科研院所基本科研业务费项目(2019JB002)。

摘　　要：鱼塘水样采用全自动在线顶空固相微萃取进行萃取:萃取温度为75℃;萃取时间为60min;氯化钠加入量为0.3kg·L^(-1);样品体积为2.0mL。采用气相色谱-串联质谱法测定水样中硫丹(α-硫丹、β-硫丹)和硫丹硫酸酯的含量,在气相色谱分离中采用DB-5ms毛细管色谱柱,在串联质谱分析中采用多反应监测模式。α-硫丹、β-硫丹和硫丹硫酸酯的质量浓度在一定范围内与其对应的峰面积呈线性关系,检出限(3S/N)为0.001~0.015μg·L^(-1),测定下限(10S/N)为0.003~0.050μg·L^(-1)。以空白水样为基体进行加标回收试验,所得回收率为83.6%~117%,测定值的日内相对标准偏差(n=6)为2.2%~18%,日间相对标准偏差(n=3)为4.2%~18%。The fishpond water samples were extracted with fully automatic online HS-SPME.Temperature of extraction was 75℃,time of extraction was 60min,adding amount of sodium chloride was 0.3kg·L^(-1)and sample volume was 2.0 mL.GC-MS/MS was applied to the determination of endosulfan(α-endosulfan andβ-endosulfan)and endosulfan sulfate in water samples.The DB-5ms capillary chromatographic column was used for GC separation and the multiple reaction monitoring mode was adopted in MS/MS determination.Linear relationships between values of peak area and mass concentration ofα-endosulfan,β-endosulfan,and endosulfan sulfate were kept in definite ranges,with detection limits(3S/N)in the range of 0.001-0.015μg·L^(-1)and lower limits of determination(10S/N)in the range of 0.003-0.050μg·L^(-1).On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 83.6%-117%,with intra-day RSDs(n=6)of determined values in the range of 2.2%-18%and inter-day RSDs(n=3)in the range of 4.2%-18%.

关 键 词：气相色谱-串联质谱法 硫丹 硫丹硫酸酯 顶空固相微萃取 全自动在线 鱼塘水 投毒案件 

分 类 号：O657.63[理学—分析化学]