固相萃取-GC／MS法测定水中有机氯农药.pdfVIP

第2O卷 第1期 环境监测管理与技术 2008年2月 · 监测技术 · 固相萃取一GC／MS法测定水中有机氯农药 杨丽莉，母应锋，胡恩宇，王丽媛 (南京市环境监测中心站，江苏 南京 210013) 摘 要：建立了固相萃取一气相色谱／质谱联用测定水中痕量六六六、滴滴涕和环氧七氯的方法。采用 c， 固相萃取柱 富集水样，二氯甲烷／丙酮混合溶剂洗脱，加入菲一d．。作为内标，利用气相色谱／质谱联用仪选择离子监测模式检测，内标法 定量，定性、定量准确，线性响应良好，干扰小，按采样 1 L计算，方法检出限为4．26 ng／L～19、2 ng／L，RSD在0、4％ 一6、3％ 之间，平均加标回收率在77．7％ ～118％之间，实际样品测定结果表明方法能满足环境水体中痕量有机氯农药的监测要求。 关键词：六六六；滴滴涕；环氧七氯；固相萃取；气相色谱／质谱联用法；水质 中图分类号：0657、7 1 文献标识码：B 文章编号：1006—2009(2008)01—0025—04 Determination of organOchlOrine Pesticides in Water Sample by Gas Chromatography·-Mass Spectrometry with Solid·-Phase Extraction YANG Li—li，MU Ying-feng，HU En—yu，WANG Li-yuan (Nanfing Environmental Monitoring Center，№njing，Jiangsu 2 1 00 1 3，China) Abstract：A method was established for trace BHC，DDT and heptachlor eqoxide in water sample by gas chromatography-mass spectrometry with solid—phase extraction．The organochlorine pesticides were extracted from water with octadecylsilica(C 18)SPE caaridge，eluted with the mixture solvent of methylene chloride and ace- tone，detected by selected ion monitoring mode and phenanthrene—d10 as internal standard．The quantity and quality method of internal standard were correct．The good linear responses were achieved and little in ference． The detection limits were 4．26 ng／L～1 9．2 ng／L when the sample yolume was 1 L and averge recoveries 77．7％ ～ 1 18％ ．RSD 0．4％ ～6．3％．The experiment results showed that the method is suitable for determination of trace organochlorine pesticides in environmental waters． Key words：BHC；DDT；Heptachlor eqoxide；Solid—phase extraction；Gas chromatography-mass spectrom- etry；Water quality 有机氯农药是人类有史以来首次发现的最强 液液萃取富集样品，有机试剂用量大，对环境和操 大的人工合成杀虫剂，在世界农业生产中长期担当 作人员危害较大，而且萃取液浓缩后用电子捕获检 防治害虫的主角。研究表明，有机氯杀虫剂虽然毒