渔业环境沉积物中硫丹及其代谢物残留的气相色谱分析

建立了渔业环境沉积物中硫丹及其代谢物硫丹硫酸酯残留量的气相色谱分析方法。样品以正已烷/丙酮(1∶1,V/V)提取、铜粉除去硫化物、石墨化碳黑-佛罗里硅土复合固相萃取柱净化、二氯甲烷/正已烷(3∶7,V/V)洗脱,用电子捕获-气相色谱(GC-ECD)测定,外标法定量。硫丹各组分在0.001～0.2μg/mL浓度范围内线性相关系良好(r≥0.9989);1、10、20μg/kg添加浓度的回收率在76.3%～107%之间,相对标准偏差(RSD)为2.31%～11.8%;α-硫丹、β-硫丹、硫丹硫酸酯的检出限(LOD)分别为0.03、0.04、0.05μg/kg(干重),最低定量限(LOQ)均为1μg/kg(干重)。适用于渔业环境硫丹污染的监测。

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.