Abstract:Gas chromatography coupled with solid-phase extraction was developed for determination of tefluthrin, bifenthrin, fenpropathrin, cyhalothrin, permethrin, cyfluthrin, cypermethrin, fenvalerate, tau-fluvalinate, and deltamethrin residues in surface sediment from aquaculture area. The pyrethroids were extracted with petroleum ether-acetone(V/V, 3∶1), followed by sulfide removal by copper powder, and purification on a carbon-florisil SPE column, then analyzed by gas chromatography with electron capture detector(GC-ECD). The linear range of tefluthrin was 2.5~100 ng/ml and the other nine prrethroids were 5~200 ng/ml(r≥0.996 7). When spiked with 2μg/kg, 20μg/kg, 40μg/kg , the average recoveries ranged from 72.8% to 107% and their relative standard deviations(RSD)were 2.75%~11.3%. The limits of detection(LOD) and quantitation( LOQ ) for all pyrethroid were in the range of 0.01~0.1μg/kg(wet weight) and 1~2μg/kg(wet weight) respectively. This method can be applied in the detection of pyrethroid residues in aquaculture area.