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

作　　者：叶玫[1] 姜琳琳[1] 余颖[1] 母玉敏[2] 

机构地区：[1]福建省水产研究所,厦门361012 [2]福建农林大学食品科学学院,福州350002

出　　处：《渔业科学进展》2012年第5期109-115,共7页Progress in Fishery Sciences

基　　金：福建省海洋与渔业厅重点项目(闽海渔合同[2009]1-17号)资助

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2.5～100ng/ml、其他9种菊酯在5～200ng/ml内线性关系良好(r≥0.9967);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0.01～0.1μg/kg(湿重),最低定量限(LOQ)为1～2μg/kg(湿重);适用于水产养殖区拟除虫菊酯污染的监测。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 2/lg/kg, 20-g/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.

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 

分 类 号：S949[农业科学—水产养殖]