A method was established for the quantitative determination of 20 organochlorine pesticides(OCPs) in crayfish by gas chromatography and mass spectrometry(GC-MS).The preparation and analytical conditions,such as extraction solvent,purification method and other analytical conditions were optimized.The samples were extracted with acetonitrile,and kept in constant volume with ethyl acetate-cyclohexane(1∶1).The extract was purified by gel permeation chromatography(GPC) combined with solid-phase extraction(SPE),and determined by GC-MS under selective ion scan(SIM) mode.Under the optimum conditions,the calibration curves of the compounds were linear in the range of 0.01-1.0 mg/L with correlation coefficients higher than 0.994,and the limits of detection(LOD,S/N=3) were in the range of 0.1-1.5 μg/kg.The recoveries of target compounds in crayfish yellow and meat samples at three spiked concentration levels of 5,10,20 μg/kg were in the range of 71.3%-117.3%,with RSDs(n=6) of 0.6%-7.5%.The method is sensitive,accurate and simple,and could be applied in the determination of 20 OCPs in crayfish. Key words:gas chromatography-mass spectrometry(GC-MS);crayfish;organochlorine pesticides(OCPs);gel permeation chromatography(GPC);solid-phase extraction(SPE);residue
关键词
气相色谱-质谱小龙虾有机氯凝胶渗透色谱固相萃取残留
Keywords
gas chromatography-mass spectrometry(GC-MS)crayfishorganochlorine pesticides(OCPs)gel permeation chromatography(GPC)solid-phase extraction(SPE)residue
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Related Institution
Key Laboratory of Tropical Fruits and Vegetables Quality and Safety for State Market Regulation;Hainan Institute for Food Control
Tea Research Institute,Chinese Academy of Agricultural Sciences
Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables;Key Laboratory of Quality and Safety Control for Subtropical Fruit and Vegetable,Ministry of Agriculture and Rural Affairs;Analysis and Test Center,Chinese Academy of Tropical Agricultural Sciences
College of Horticulture and Landscape,Tianjin Agricultural University