气相色谱-电子捕获检测法和气相色谱-质谱法同时测定鱼体内19种有机氯农药

Simultaneous Determination of 19 Organochlorine Pesticides in Fish Using Gas Chromatography and Gas Chromatography-Ion Trap Mass Spectrometry Confirmation

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.