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
Keywords
organophosphoruspesticide residuesgel permeation chromatographysolid phase extractiongas chromatographyFruit traditional Chinese medicines
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Related Institution
Guangdong Provincial Engineering Research Center for Quality and Safety of Traditional Chinese Medicine,Guangdong Provincial Key Laboratory of Chemical Measurement and Emergency Test Technology, Institute of Analysis,Guangdong Academy of Sciences(China National Analytical Center,)