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

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.