| 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。 |
| 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 |
| DOI： |
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| 基金项目:福建省海洋与渔业厅重点项目（闽海渔合同[2009]1-17 号） |
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| Determination of pyrethroids residue in surface sediment from aquaculture area by gas chromatography |
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| 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． |
| Key words: Pyrethroid Residue Gas chromatography Surface sediment Aquaculture area |
