液相色谱-串联质谱法测定蔬菜、水果中80种农药残留  

Determination of 80 Pesticide Residues in Vegetables and Fruits by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：曹赵云[1] 牟仁祥[1] 应兴华[1] 林晓燕[1] 陈铭学[1] 

机构地区：[1]中国水稻研究所农业部稻米及制品质量监督检验测试中心,浙江杭州310006

出　　处：《分析测试学报》2010年第10期1030-1035,共6页Journal of Instrumental Analysis

摘　　要：建立了同时测定蔬菜、水果中有机磷类、酰胺类、氨基甲酸酯类等80种农药残留的液相色谱-串联质谱(LC-MS/MS)检测方法。样品经乙腈提取,N-丙基乙二胺(PSA)和C18填料分散固相萃取净化,C18柱分离后,在电喷雾正离子化模式下,于三重四极杆质谱仪,动态多反应监测方式测定。结果表明:80种农药的线性范围均超过3个数量级,且r≥0.99;对6种蔬菜、水果样品分别进行0.01、0.05mg/kg2个水平的加标回收实验(n=5),其平均回收率分别为64%～118%和72～108%;RSD分别为3.7%～29.1%和3.4%～27.9%;80种农药的方法检出限(S/N=3)为0.02～3μg/kg。方法快速、准确、灵敏,适用于蔬菜、水果中该80种农药的同时分析。A liquid chromatography-tandem mass spectrometric（LC-MS/MS）method was developed for the simultaneous determination of 80 pesticides of different chemical classes（mainly including organophosphorous compounds,acetanilide herbicide and carbamates）in vegetables and fruits.The sample was extracted with acetonitrile,and cleaned up by PSA and C18 columns.80 pesticides were separated on a C18 column（1.8 μm,100 mm×2.1 mm i.d.）using 0.1% formic acid and 5 mmol/L ammonium acetate in water（A）-acetonitrile（B）as mobile phase in gradient elution.The analytes were detected with positive-ion electrospray ionization-mass spectrometry in dynamic multiple reaction monitoring（Dynamic MRM）mode.Under the optimal conditions,the linear ranges for all the pesticides were over 3 orders of magnitude with correlation coefficients not less than 0.99.The detection limits（LODs）ranged from 0.02 to 3 μg/kg（S/N=3）.The recoveries of 80 pesticides were measured from samples of different fruits and vegetables.The results showed that the mean recoveries of 80 pesticide residues at two spiked concentration levels of 0.01 and 0.05 mg/kg were in the range of 64%-118% and 72%-108%,respectively,with relative standard deviations（RSDs）of 3.7%-29.1% and 3.4%-27.9%,respectively.The method was rapid,sensitive,reliable,and could be used to analyse the pesticide residues in a wide variety of fruits and vegetables.

关 键 词：液相色谱-串联质谱 多农药残留 蔬菜 水果 

分 类 号：O657.72[理学—分析化学] F767.2[理学—化学]