气相色谱-串联质谱法同时测定水体和底泥中多氯联苯及有机氯农药残留  

Simultaneous determination of polychlorinated biphenyl and organochlorine pesticides residues in water and sediment by gas chromatography-tandem mass spectrometry

作　　者：彭婕[1] 陈建武[1] 甘金华[1,2] 居小倩 伍刚 何力[1,2] PENG Jie;CHEN Jianwu;GAN Jinhua;JU Xiaoqian;WU Gang;HE Li(Yangtze River Fisheries Research Institute,Chinese Academy of Fishery Sciences,Fishery Quality Supervision and Testing Center of Ministry of Agriculture and Rural Affairs,Fishery Products Quality Safety Risk Assessment Laboratory(Wuhan)of Ministry of Agriculture and Rural Affairs,Wuhan,430223,China;Key Laboratory of Control of Quality and Safety for Aquatic Products of Ministry of Agriculture and Rural Affairs,Beijing,100141,China)

机构地区：[1]中国水产科学研究院长江水产研究所农业农村部淡水鱼类种质监督检验测试中心农业农村部水产品质量安全风险评估实验室(武汉),武汉430223 [2]农业农村部水产品质量安全控制重点实验室,北京100141

出　　处：《环境化学》2020年第8期2307-2316,共10页Environmental Chemistry

基　　金：中央级公益性科研院所基本科研业务费专项资金(2018JBF);现代农业产业技术体系专项资金(CARS-48);中国水产科学研究院基本科研业务费(2018HY-ZD0603);国家农产品质量安全风险评估项目(GJFP2019032)资助

摘　　要：建立了气相色谱-串联质谱(GC-MS/MS)同时测定水体和底泥中7种指示性多氯联苯和19种有机氯农药残留的分析方法.水样由二氯甲烷萃取,弗罗里硅土固相萃取柱净化;底泥样品经二氯甲烷-正己烷(1∶1,V/V)超声提取,氨基固相萃取柱净化.采用TG-5MS(30 m×0.25 mm×0.25μm)色谱柱对目标物进行分离,在电子轰击电离源下以选择反应监测模式(SRM)进行检测.结果表明,26种目标物在1.00—200μg·L-1线性范围内线性关系良好,相关系数均大于0.994.空白水样中低、中、高的3个添加浓度下的平均加标回收率为66.1%—109.1%,相对标准偏差(RSD)为2.3%—10.9%,检出限(LOD)为0.24—0.60 ng·L-1.空白底泥样品中低、中、高的3个添加浓度下的平均加标回收率为69.8%—109.9%,RSD为2.0%—11.3%,检出限(LOD)为0.06—0.15μg·kg-1.该方法选择性好、灵敏度高、重现性好,能够满足水体和底泥中多种多氯联苯和有机氯农药残留的检测要求.A method based on gas chromatography-tandem mass spectrometry(GC-MS/MS)was developed for the simultaneous determination of seven polychlorinated biphenyl(PCBs)and nineteen organochlorine pesticides(OCPs)residues in water and sediment samples.The water samples were extracted with dichloromethane and cleaned up by florisil solid-phase extraction columns.The sediment samples were extracted with dichloromethane-hexane(1∶1,V/V)by ultrasonic wave.Then the extracts were further purified with aminopropyl cartridge.The purified solutions were isolated by TG-5 MS column(30 m×0.25 mm×0.25μm)and detected using selective reaction monitoring(SRM)mode at the electron impact source.It was observed that this method had good linearity in the range of 1.00—200μg·L-1 for the 26 analytes,and the correlation coefficients were all higher than 0.994.Average recoveries of 26 analytes in the blank water samples,which were spiked at three concentration levels,were between 66.1%and 109.1%,with RSDs of 2.3%—10.9%.The limit of detection(LOD)were 0.24—0.60 ng·L-1.The average recoveries of 26 analytes in the blank sediment samples at three spiked levels ranged from 69.8%to 109.9%with RSDs of 2.0%—11.3%.The LOD were 0.06—0.15μg·kg-1.This method was suitable for the determination of seven polychlorinated biphenyl and nineteen organochlorine pesticides residues in aquatic environmental water and sediment with high sensitivity and selectivity.

关 键 词：气相色谱-串联质谱(GC-MS/MS) 多氯联苯 有机氯农药 水体 底泥 

分 类 号：O657.63[理学—分析化学] X830.2[理学—化学]