气相色谱法测定水产养殖区表层沉积物中拟除虫菊酯残留量

Determination of pyrethroids residue in surface sediment from aquaculture area by gas chromatography

关键词:  拟除虫菊酯  残留  气相色谱法  表层沉积物  水产养殖区

Key words:  Pyrethroid  Residue  Gas chromatography  Surface sediment  Aquaculture area

摘要:

建立了固相萃取-气相色谱法测定水产养殖区表层沉积物中七氟菊酯、联苯菊酯、甲氰菊酯、三氟氯氰菊酯、氯菊酯、氟氯氰菊酯、氯氰菊酯、氰戊菊酯、氟胺氰菊酯、溴氰菊酯10种拟除虫菊酯残留的分析方法。样品以石油醚/丙酮（V/V，3∶1）提取、铜粉除去硫化物、石墨化碳黑-佛罗里土复合固相萃取柱净化、石油醚/丙酮（V/V，4∶1）洗脱、电子捕获-气相色谱测定, 外标法定量。七氟菊酯在2.5～100 ng/ml、其他9种菊酯在5～200 ng/ml内线性关系良好(r≥0.996 7)；2、20、40μg/kg添加浓度的回收率在72.8%～107%之间，相对标准偏差（RSD）为2.75%～11.3%；检出限（LOD）为0.01～0.1 μg/kg（湿重），最低定量限（LOQ）为1～2 μg/kg（湿重）；适用于水产养殖区拟除虫菊酯污染的监测。

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．