分散固相萃取-反相高效液相色谱法测定蔬菜、水果中10种氨基甲酸酯类农药残留  

Simultaneous Determination of Ten Carbamate Pesticide Residues in Vegetables and Fruits with Dispersive Solid Phase Extraction Cleanup and Reverse Phase High Performance Liquid Chromatography

作　　者：丁晨红[1] 骆冲[1] 邓义才[1] 王富华[1] 王刚[1] 叶倩[1] 梁应坤 

机构地区：[1]广东省农业科学院农产品公共监测中心,广东广州510640

出　　处：《热带农业科学》2014年第4期77-82,共6页Chinese Journal of Tropical Agriculture

摘　　要：建立分散固相萃取-反相高效液相色谱同时测定蔬菜和水果中10种氨基甲酸酯类农药（涕灭威，涕灭威砜，涕灭威亚砜，克百威，3-羟基克百威，灭多威，甲萘威，异丙威，速灭威，仲丁威）残留的分析方法。样品经乙腈提取， PSA分散固相萃取净化，液相色谱柱后衍生分离，荧光检测（姿ex＝330 nm,姿em＝465 nm）测定，外标法定量。10种农药在0.005～0.50 mg/L范围内线性关系良好；检出限在0.004～0.008 mg/L；平均加标回收率在75.6%～112.3%，相对标准偏差（RSD）在0.8%～10.2%。该方法具有快速、灵敏、准确、重现性好以及操作简单等特点，适合日常大批量蔬菜和水果样品中10种氨基甲酸酯类农药残留的测定。Developed a method for the simultaneous determination of ten pesticide residues including aldicarb, aldicarb sulfone, aldicarb sulfoxide, methomyl, carbofuran, 3-hydroxycarbofuran, carbaryl,isoprocarb, metolcarb, fenobucarb in vegetables and fruits by Dispersive solid-phase extraction cleanup and Phase High Performance Liquid Chromatography-Fluorescence Detector （HPLC-FLD）. The sample was extracted by acetonitrile and purified by Primary-secondary amine （PSA） dispersive solid phase extraction. The collected solution was analyzed by HPLC-FLD with post-column derivation and quantified by external standard method. The wavelengths were set at 330 nm and 465 nm. The results indicated that the calibration curves of the ten pesticides showed good linear relationship in the concentration of 0.005~0.50 mg/L with correlation coefficients greater than 0.999. The detection limits ranged from 0.004~0.008 mg/L. The recoveries ranged from 75.6%~112.3%with the relative standard deviation （RSD） range of 0.8%~10.2%. The method was simple, rapid, sensitive, accurate, and was suitable for the determination of the above 10 pesticide residues in fruits and vegetables.

关 键 词：分散固相萃取 反相高效液相色谱法 荧光检测 氨基甲酸酯 农药残留 

分 类 号：O657.72[理学—分析化学]