固相萃取-气质联用法测定水中三氯杀螨醇及百菌清

Determination of dicofol and chlorothalonile pesticide residues in water by gas chromatography-mass spectrometry with solid phase extraction

目的:建立了水中多种拟除虫菊酯类农药残留的固相萃取-气相色谱-质谱(GC/MS)联用检测方法。方法:采用C18固相萃取碟富集吸附水样中目标组分,以二氯甲烷洗脱浓缩; DB-5MS毛细管柱分离,采用选择离子监测SIM的质谱扫描模式进行定性定量分析。结果:在50~400μg/L浓度范围内线性关系良好,相关系数均>0 .995,三氯杀螨醇、百菌清加标平均回收率为90 .0% ~101 .1%,方法的相对标准偏差为4. 2% ~8. 3%,水样浓缩2 .500倍的最低检测限分别为0 .0012、0. 0024μg/L。结论:本法具有非常高的选择性、灵敏度和准确度,完全能满足水中痕量三氯杀螨醇及百菌清的分析。

Objective:To establish a Gas Chromatography-Mass Spectrometry method for the determination of dicofol and chlorothalonile in water using solid phase extraction.Methods:Wate sample was extracted on C_(18) solid phase disk and eluted with dichloromethane, then separated by GC with an DB-5MS capillary column. The interest analytes were identified and quantified by SIM mode.Results:Good linearity which correlation coefficent was greater than 0.995 was observed between 50^(400 μg/L).The average recoveries of Dicofol and Chlorothalonile ranged from 90.0%~101.1% and their relative standard deviation varied between 4.2% and 8.3%. Detection limit of each component diluted 2 500 times was 0.0012,0.0024 μg/L, respectively.Conclusion:The method established was so selective and sensitive and exact that it can be applied to high sensitive analysis for dicofol and chlorothalonile pesticides in water.