固相膜萃取-高效液相色谱法测定饮用水中12种氨基甲酸酯类农药残留

Determination of twelve carbamate residues in drinking water by HPLC after solid-phase membrane extraction

目的:建立固相膜萃取-高效液相色谱法测定饮用水中灭多威、涕灭威、速灭威、残灭威、呋喃丹、甲萘威、抗杀虫威、异丙威、硫双威、仲丁威、猛杀威、杀虫威等12种氨基甲酸酯类农药残留量的方法。方法:水样经C18固相萃取膜真空抽滤,滤膜用乙酸乙酯洗脱,洗脱液经氮吹、甲醇溶解,高效液相色谱法测定。结果:12种氨基甲酸酯类农药的线性范围为0.05 mg/L～25.0 mg/L,线性相关系数大于0.999,检出限为0.31 mg/L～1.25 mg/L,水样中氨基甲酸酯类农残最低检测浓度范围为0.005 mg/L～0.019 mg/L,加标回收率为59.3%～97.3%,RSD<7.5%。结论:本方法样品前处理方便、快捷,有机试剂用量少。

Objective：To establish a method for determination of 12 carbamate residues including methomyl,aldicarb,metolcarb,profluoralin,furadan,methyl carbamate,pirimicarb,isoprocarb,thiodicarb,fenobucarb,promecarb and tetrachlorvinphose in drinking-water by high performance liquid chromatography after solid-phase membrane extraction.Methods： The water sample was filtered through the conditioned solid-phase membrane under vacuum.The carbamates absorbed on the membrane were eluted using ethyl acetate and the eluted solution was blown to dryness under nitrogen gas.The residue was reconstituted with methanol and analyzed by HPLC.Results： The linear range of 12 carbamates residues were between 0.05 mg/L to 25.0 mg/L with r0.999.The detection limits were 0.31 mg/L to 1.25 mg/L.The lowest detection limits of carbamate residues in the sample water were between 0.005 mg/L and 0.019 mg/L.The recoveries ranged from 59.3% to 97.3% with RSD7.5%.Conclusion： The method can be used for the multi-residue analysis of carbamate residues in drinking water.