果实类中药材中20种有机磷农药残留量的同时测定  

Simultaneous Determination of 20 Kinds of Organophosphorus Pesticide Residues in Fruit Traditional Chinese Medicines

作　　者：王均[1] 曹淑瑞[2] 张雷[2] 徐芬[2] 王国民[2] 李贤良[2] 

机构地区：[1]重庆医科大学药学院,重庆400016 [2]重庆出入境检验检疫局,重庆400020

出　　处：《分析测试学报》2013年第11期1309-1315,共7页Journal of Instrumental Analysis

基　　金：质检公益性行业科研专项资助项目(201010045)

摘　　要：建立了果实类中药材中多种有机磷农药残留同时测定的方法,并对影响提取、净化、检测效率的因素进行优化。样品用乙酸乙酯提取，凝胶渗透色谱收集9-15 min流分，ENVI-Carb固相萃取柱净化，DB-1701毛细管色谱柱分离，火焰光度检测器检测，外标法定量。在优化条件下，20种有机磷农药在0.01-2.0 mg/L 范围内具有良好的线性关系，相关系数为0.996 6-0.999 5，检出限（S/N=3）为0.66-5.78 μg/kg。3个加标水平下的平均回收率为80.2%-109.9%，相对标准偏差为2.3%-13%。该方法操作简便、准确、净化效果好，可满足果实类中药材中多种有机磷农药残留的同时测定要求。A gas chromatographic method was established for the simultaneous determination of 20 kinds of organophosphorus pesticide residues,including dichlorvos,methamidophos,acephate,cadusafos,phorate,omethoate,fonofos,dimethoate,pirimiphos-methyl,chlorpyrifos,malathion,fenthion,isofenphos methyl,fenitrothion,parathion,isocarbophos,profenofos,fenamiphos,triazophos and pyridaphenthion,in Fruit traditional Chinese medicines（Dried tangerine peel,Foeniculum vulgare,Jave amonum fruit,Fructus arctii,Lycium chinense,Dried red dates）.The factors affecting the extraction,purification,detection efficiency were optimized,and the optimal conditions were as the following：the samples were extracted with ethyl acetate,and the elution fractions of gel permeation chromatography was collected at 9-15 min,then purified with ENVI-Carb solid phase extraction column.The separation of target compounds were performed on a film thickness of DB-1701 capillary column（30 m×0.25 mm×0.25 μm）,and the quantitative analysis of organophosphorus pesticides was carried out by gas chromatography with flame photometric detector and the external standard method.Under the optimized conditions,the calibration curves of 20 organophosphorus pesticides were linear in the range of 0.01-2.0 mg/L with correlation coefficients of 0.996 6- 0.999 5.The detection limits（S/N=3） were in the range of 0.66-5.78 μg/kg.The recoveries of the pesticides in various Fruit traditional Chinese medicines at three spiked levels ranged from 80.2% to 109.9%,with relative standard deviations of 2.3%-13%.With the advantages of easy operation,accuracy and sensitivity,the method is applicable in the simultaneous determination of 20 kinds of organophosphorus pesticide residues in Fruit traditional Chinese medicines.

关 键 词：有机磷 农药残留 凝胶渗透色谱 固相萃取 气相色谱 果实类中药材 

分 类 号：O657.7[理学—分析化学] F767.2[理学—化学]