食品中常见有机磷农药残留的气相色谱-质谱检测方法  

Detection of organophosphorus pesticide residues in food by gas chromatography-mass spectrometry

作　　者：崔如玉 李壹[1] 熊晓辉[1] 

机构地区：[1]南京工业大学食品与轻工学院,江苏南京211800

出　　处：《南京工业大学学报（自然科学版）》2017年第1期137-144,152,共9页Journal of Nanjing Tech University(Natural Science Edition)

基　　金：国家科技支撑计划(2012BAK17B09);江苏省科技基础设施建设计划(BM2012026)

摘　　要：建立了气相色谱-质谱联用技术分析蔬菜、谷物中敌敌畏、甲胺磷等16种有机磷农药残留的快速检测方法。样品用乙腈提取,采用Qu ECh ERS处理方法进行前处理,用气相色谱-质谱联用多反应监测仪检测16种有机磷农药残留。16种有机磷农药在15 min内流出,分离度良好,农药在0.025~0.4 mg/kg范围内线性良好,相关系数(R2)均大于0.94。不同基质如大米、面粉、蔬菜的加标回收率分别为75.9%~112.2%、77.3%~126.9%、76.2%~125.3%,相对标准偏差(RSD)<8.5%。重复性实验引入的不确定度符合国家标准。该方法具有操作方便、分离时间短、灵敏度高、选择性好等优点,适用于大多数食品中有机磷农药残留检测。To establish a rapid detection method for the determination of dichlorvos,methamidophos and other organophosphorus pesticide residues in vegetables and grains by gas chromatography-mass spectrometry （ GC-MS ）,samples were first extracted with acetonitrile and pretreated by QuEChERS method,then detected by gas chromatography-mass spectrometry under multiple reaction monitoring. 16 kinds of organophosphorus pesticides could be detected within 15 min with a good separating degree and good linearity. T he correlation coefficient range was 0. 025-0. 4 mg /k g,and the correlation coefficient （fi2） were more than 0. 94.The standard addition recovery rates of different substrates such as rice, flour, and vegetable were in the ranges of 75. 9%-112. 2%, 77. 3%-126. 9%, and 76. 2%-125. 3 % with relative standard deviation （RSD ） 〈 8. 5% . The uncertainty of the repeated experiments met the national standards. T he method was simple, rapid,high sensitivity,good selectivity,and was suitable for determination of organophosphorus pesticides residues in food.

关 键 词：气相色谱-质谱仪 有机磷 农药残留 食品 

分 类 号：O657.63[理学—分析化学]