摘要
建立了气相色谱-电子捕获检测(GC-ECD)法同时测定,及气相色谱-离子阱-多级质谱(GC-IT-MS/MS)法定量确证鱼体中19种有机氯农药(OCPs)残留的检测方法。目标物采用浸渍-振荡法提取,固相萃取(SPE)(脂肪含量≤1.0%)和凝胶色谱(GPC)净化,浓缩,定容后上机测定。草鱼肌肉空白组织中目标化合物的添加浓度为2.0、5.0μg/kg时,GC-ECD法与GC-IT-MS/MS法的回收率分别为72.8%~96%和78.8%~106%,相对标准偏差分别为2.1%~14.9%和4.8%~11%。定量限(S/N=10)分别为0.07~1.44μg/kg和0.10~4.27μg/kg。本方法已成功应用于长江圆口铜鱼体中多种OCPs残留的同时测定。
A method was proposed for the simultaneous determination of 19 organochlorine pesticides(OCPs)in fish by gas chromatography with electron capture detection(GC-ECD)and gas chromatography-ion trap mass spectrometry.After extraction by a high-speed homogenizer using a mixture of acetone and hexane(1∶1,V/V)as the solvent,the samples were clean-up by gel permeation chromatography(GPC)or solid phase extraction(SPE)(fatty≤1.0%),and followed by analysis using GC-ECD/GC-MS.At spiked level of 2 μg/kg and 5 μg/kg for 19 OCPs,recoveries were 72.8%~96% and 78.8%~106%,with a relative standard deviation(RSD)ranging from 2.1%~14.9% and 4.8%~11%.LOQ(S/N=10)were between 0.07~1.44 μg/kg and 0.10~4.27 μg/kg for the GC-ECD and GC-IT-MS/MS,respectively.The method is sensitive and can be effectively used to simultaneously quantify trace levels of many classes of organochlorine pesticides in Bronze gudgeon form Yichang reaches of the Yangtze river.
出处
《分析科学学报》
CAS
CSCD
北大核心
2010年第5期497-502,共6页
Journal of Analytical Science
基金
中国水产科学研究院内陆渔业生态环境和资源重点开放实验室基金(No.YM2007-04)
关键词
多残留同时分析
鱼
有机氯农药
气相色谱-电子捕获检测
气相色谱-质谱
Simultaneous determination
Fish
Organochlorine pesticides
Gas chromatography-electron capture detection
Gas chromatography-ion trap mass spectrometry