Analysis of endosulfan and its metabolite residues in sediment from fisheries environment by gas chromatography

A method was developed for the determining of endosulfan and its metabolite residues in sediment from fisheries environment by gas chromatography.The samples were extracted with n-hexane/acetone(1∶ 1,V/V),sulfide were removed by copper powder,and purified on a carbon-florisil SPE column eluted with dichloromethane/n-hexane/acetone(3∶ 7,V/V),then analyzed by gas chromatography with electron capture detector(GC-ECD) using the external standard.The linear range of each endosulfan derivative were 0.001~0.2 μg/mL(r≥0.9989).When spiked with 1,10,20 μg/kg,the average recoveries ranged from 76.3% to 107% and their relative standard deviations(RSD)were between 2.31% and 11.8%.The limits of detection(LOD) of α-endosulfan,β-endosulfan and endosulfan sulfate were 0.03,0.04,0.05 μg/kg(dry weight) respectively,while the limit of quantization(LOQ) was 1 μg/kg(dry weight) for all of them.This method can be applied in the detection of endosulfan contamination in fisheries environment.