液相色谱-串联质谱法测定食用菌中20种农药残留  

Determination of 20 Pesticide Residues in Edible Fungi by Liquid ChromatographyTandem Mass Spectrometry

作　　者：陈舒奕 钟茂生 江晓芬 朱品玲 梁剑 叶洪 肖颖 

机构地区：[1]宁德出入境检验检疫局,福建宁德352100 [2]莆田出入境检验检疫局,福建莆田351100

出　　处：《福建农业学报》2016年第12期1334-1339,共6页Fujian Journal of Agricultural Sciences

基　　金：福建出入境检验检疫局科研项目(FK2014-ND002)

摘　　要：本研究建立了食用菌中20种农药残留同时检测的液相色谱-串联质谱（LC-MS/MS）检测方法。样品经含0.1%乙酸的乙腈提取,经无水硫酸镁、N-丙基乙二胺（PSA）净化,以电喷雾电离正离子（ESI＋）、多反应检测模式（MRM）进行检测,外标法定量。20种农药在0.005-0.10mg·kg^-1范围内线性关系良好,相关系数大于0.99。该分析方法快速、准确,通过优化前处理和上机条件,在最优条件下进行测试,方法定量下限（S/N〉10）为0.005mg·kg^-1,在香菇和白木耳中进行0.05 mg·kg^-1加标水平测试,其回收率为65.1%-96.0%,RSD为2.5%-9.0%。该方法适用于食用菌中20种农药测定。A method by combining liquid chromatography with tandem mass spectrometry was developed to determine the residues of 20 pesticides in edible fungi.Samples were extracted using acetonitrile containing 0.1%acetic acid cleaned-up with anhydrous magnesium sulfate and primary secondary amine（PSA）.Measurement on the residues was conducted on the extracts under the modes of electrospray positive ionization（ESI＋）and multiple reaction monitoring（MRM）,using external standards.The calibration curves of the pesticides had a linear relationship with a correlation coefficients greater than 0.99 in the range of 0.005 to 0.10mg·kg^-1.The optimized testing conditions included a lower limits of quantitation（LOQs,S/N10）at 0.005mg·kg^-1.A test for recovery was performed by adding 0.05mg·kg^-1 standard pesticides to the mushrooms and white fungi.It was found that the recovery rates ranged from 65.1% to 96.0%,with a relative standard deviations of 2.5%-9.0%.It was concluded that the newly developed methodology was rapid and accurate,and could be applied for the determination of the 20 pesticide residues in edible fungi.

关 键 词：液相色谱-串联质谱法 食用菌 农药残留 

分 类 号：O657[理学—分析化学]