Determination of OCPs in Crayfish by GPC-SPE/GC-MS

KeyWord:gas chromatography-mass spectrometry(GC-MS)  crayfish  organochlorine pesticides(OCPs)  gel permeation chromatography(GPC)  solid-phase extraction(SPE)  residue

Abstract:

      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¡Ã1).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 ¦Ìg/kg£®The recoveries of target compounds in crayfish yellow and meat samples at three spiked concentration levels of 5£¬10£¬20 ¦Ìg/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£ºgas chromatography-mass spectrometry(GC-MS)£»crayfish£»organochlorine pesticides(OCPs)£»gel permeation chromatography(GPC)£»solid-phase extraction(SPE)£»residue