凝胶净化气相色谱-质谱选择离子测定蔬菜水果中多种农药残留  

Determination of multiresidue pesticides in vegetables and fruits by gel-permeation cleanup and gas chromatography/mass spectrometry

作　　者：曹艳平[1] 李蔚[1] 李凤华[1] 

机构地区：[1]山东省疾病预防控制中心,济南250014

出　　处：《中国卫生检验杂志》2010年第12期3207-3209,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的:建立一种测定蔬菜水果中有机磷、氨基甲酸酯、除虫菊酯和有机氯类多种农药残留的气相色谱质谱分析方法。方法:采用乙腈超声提取蔬菜水果中多种农药,以全自动凝胶净化、自动浓缩后,用气相色谱-质谱选择离子监测方式分析检测18种有机磷、7种氨基甲酸酯、8种除虫菊酯类、1种有机氯农药残留。结果:所有34种农药均在45 min内流出,分离良好,农药标准的线性范围在0.003μg/ml～10μg/ml,相关系数r均在0.99以上,低、高二种浓度加标回收率均在55.3%～128.1%之间,相对标准偏差均小于20%,方法最低检出限在0.006 mg/kg～0.05 mg/kg(S/N?3)。结论:方法适合于蔬菜和水果中有机磷、氨基甲酸酯、除虫菊酯和有机氯类农药的测定。Objective：To establish a method for determination of organophosphorus,carbamate,pyrethroid,organochlorine pesticides in vegetables and fruits by gas chromatography/mass spectrometry（GC/MS） and selected ion monitoring（SIM）.Methods： The pesticides were extracted with acetonitrile by ultrasonic wave.The extract was cleaned-up by Auto-Gel-Permeation Cleanup（GPC）.The analysis was performed by gas chromatography/mass spectrometry（GC/MS） and selected ion monitoring（SIM）.Retention time and specific ions were used to confirm the pesticides.Results： The calibration curves of 34 pesticides were linear（correlatiom coefficient r0.99） within the range of 0.003 μg/ml～10 μg/ml.The recoveries were ranged from 55.3%～128.1%,the relative standard deviations（RSD） of the method was 20% for each case,and the limit of determination（LOD）,defined in terms of 3 times baseline noise was 0.006 mg/kg～0.05 mg/kg.Conclusion： The method is suitable for determining pesticides in fruits and vegetables.

关 键 词：蔬菜和水果 有机磷、氨基甲酸酯、除虫菊酯和有机氯类农药 凝胶净化 气相色谱-质谱分析 选择离子监测方式 

分 类 号：O657.63[理学—分析化学]