食品中33种残留农药的液质联用一次测定法  

Determination of 33 Kinds of Pesticide Residues in Food by Liquid Chromatography-Mass Spectrometry

作　　者：于维森[1] 王孝钢[2] 于红卫[1] 饶小思[1] 

机构地区：[1]山东省青岛市疾病预防控制中心理化检验科,266033 [2]农业部农产品质量监督检验测试中心

出　　处：《职业与健康》2011年第5期512-514,共3页Occupation and Health

基　　金：国家"十一五"科技支撑计划项目--重大活动中食品安全保障技术研究与示范(2006BAK02A27);青岛市科技局立项课题(06-3-2-2nsh)

摘　　要：目的建立一种测定食品中农药残留的液相色谱质谱方法。方法采用乙腈匀浆提取,盐析离心后,经固相萃取柱净化,用乙腈+甲苯(3+1)洗脱农药,根据不同检测要求用液相色谱-质谱联用仪检测农药多残留组分。结果所有33种农药均在40 min内流出,农药标准的线性范围在0.01～1.0μg/ml,相关系数r均在0.99以上,低、高2种浓度加标回收率均在81%～95%之间,相对标准偏差均小于10%,方法最低检出限在0.001～0.04 mg/kg(S/N=3)。结论方法选择性强,适合于食品中有机磷、有机氯、拟除虫菊酯、氨基甲酸酯、除草剂农药残留的测定,且准确度好,精密度高,可快速一次检测33种农药,达到残留量检测中所要求的检测浓度水平。[Objective]To establish a method for determination of pesticide residues in foods by liquid chromatography-mass spectrometry（LC-MS）. [Methods]The pesticide residues were extracted with acetonitrile homogenate,purified by SPE cartridge,then eluted with acetonitrile and toluene（3＋1）.Afterwards,liquid chromatography mass spectrometry（LC-MS） was used to determine pesticide residues ingredients according to the different requirements. [Results]All the 33 kinds of pesticide residues were drained out within 40minutes;the standard linear range was between 0.01~1.0 μg/ml;correlation coefficient r was above 0.99;the labeled recovery rates of low and high concentration were both between 81%~95%;the relative standard deviations was below 10%;the limit of determination was 0.001~0.04 mg/kg（S/N=3）. [Conclusion]This method is suitable for determining pesticide residues of organophosphate,organochlorine,pyrethroid,carbamate,herbicides in foods with satisfactory selectivity,accuracy and precision;it can rapidly detect 33 kinds of pesticide and the concentration level meets the requirement for detection.

关 键 词：食品 农药 液相色谱-质谱分析 选择离子监测方式 

分 类 号：R115[医药卫生—公共卫生与预防医学]