固相萃取-GC/MS法测定水样中20种有机氯农药

Determination of Organochlorine Pesticides in Water Sample by Gas Chromatography-Mass Spectrometry Coupled with Solid-Phase Extraction

摘要: 建立了用固相萃取小柱提取和净化、GC/MS定性定量同时测定水样中20种有机氯农药的方法。方法采用OasisHLB固相萃取小柱萃取富集水样，二氯甲烷洗脱，加入菲-d₁₀作为内标，利用GC/MS进行定性定量，步骤简便，线性响应良好，干扰小，方法检出限为0.21～0.72 ng/L（按水样1L计），加标回收率为64.8%～122%，RSD为1.2%～11.0 %。成功利用该方法对广西实际河水样品进行了检测。结果表明方法可以同时满足环境水样中20种痕量有机氯农药的测定。

Abstract: A gas chromatography-mass spectrometry coupled with solid-phase extraction method has been established to determine 20 Organochlorine pesticides in water samples. Organochlorine pesticides were extracted from water with OasisHLB SPE cartridge,eluted with methylene chloride,detected in a selected ion monitoring mode with phenanthrene-d₁₀ as the internal standard.Good linear responses and little interference were achieved. The method detection limits ranged from0.21ng/Lto0.72ng/L when the sample volume was1L.The recoveries were 64.8%～122% (n=6) with RSDs of 1.2%～11.0%. This method has been successfully applied to the determination of organochlorine pesticides in river water samples obtained from Guangxi and is suitable for the analysis of organochlorine pesticides of low concentration levels in water samples.