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微波辅助萃取/气相色谱-质谱联用分析蔬菜中的有机磷农药
引用本文:杨云,张卓旻,李攻科.微波辅助萃取/气相色谱-质谱联用分析蔬菜中的有机磷农药[J].色谱,2002,20(5):390-393.
作者姓名:杨云  张卓旻  李攻科
作者单位:中山大学化学与化学工程学院,广东,广州,510275
基金项目:国家重点基础研究发展规划项目 (G2 0 0 0 0 2 6 30 2 ),教育部留学回国人员科研启动基金项目
摘    要:建立了微波辅助萃取(MAE)/气相色谱-质谱联用法(GC-MS)测定蔬菜样品中二嗪磷、水胺硫磷的分析方法,研究了不同溶剂的萃取效率。选择二氯甲烷为萃取溶剂,采用二因素三水平的正交设计实验优化了萃取溶剂体积和萃取时间。方法的线性范围分别为二嗪磷和对硫磷4ng/g-400ng/g,水胺硫磷20ng/g-400ng/g,检出限分别为二嗪磷和对硫磷4ng/g-400ng/g、水胺硫磷20ng/g-400ng/g,检出限分别为二嗪磷0.29ng/g、对硫磷1.70ng/g、水胺硫磷2.30ng/g。测定200.0ng/g和50.0ng/g加标蔬菜样品,回收率为72.2%-102.0%,RSD为1.5%-11.0%。与传统的机械振荡萃取法相比,不仅萃取效率相当,而且还具有省时省溶剂的优点。

关 键 词:分析  蔬菜  微波辐助萃取  气相色谱-质谱  有机磷农药  联合技术  食品
文章编号:1000-8713(2002)05-0390-04
修稿时间:2002年6月26日

Determination of Organophosphorus Pesticides in Vegetables by Microwave-Assisted Extraction/Gas Chromatography-Mass Spectrometry
YANG Yun,ZHANG Zhuo min,LI Gong ke.Determination of Organophosphorus Pesticides in Vegetables by Microwave-Assisted Extraction/Gas Chromatography-Mass Spectrometry[J].Chinese Journal of Chromatography,2002,20(5):390-393.
Authors:YANG Yun  ZHANG Zhuo min  LI Gong ke
Institution:Chemistry and Chemical Engineering School, Sun Yat-sen University, Guangzhou, China.
Abstract:A method of microwave assisted extraction (MAE) followed by gas chromatography mass spectrometry (GC MS) for the determination of organophosphorus pesticides (OPPs) in vegetables has been developed. The OPPs studied were diazinon, parathion and isocarbophos. Several extraction solvents were compared on the MAE efficiency. Dichloromethane gave good recovery, and was chosen for the procedure. A three level orthogonal array design was used to optimize the MAE process. Factors affecting the MAE efficiency were considered, including the solvent amount and extraction time. The linear ranges of the method were from 4 ng/g to 400 ng/g for diazinon and parathion, and from 20 ng/g to 400 ng/g for isocarbophos. The detection limits were 0 29 ng/g , 1 70 ng/g and 2 30 ng/g for diazinon, parathion and isocarbophos respectively. Two sets of spiked vegetable samples of 200 0 ng/g and 50 0 ng/g were determined. The recoveries were from 72 2% to 102 0%, and the RSDs were from 1 5% to 11 0% ( n =3). The analytical results agreed quite well with those obtained by conventional extraction with mechanical shaking (EMS). The method is fast and solvent saving.
Keywords:microwave  assisted extraction  gas chromatography  mass spectrometry  organophosphorus pesticide
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