QuEChERS结合超高效液相色谱质谱法测定禽蛋及其制品中42种农药及其代谢物  

Determination of 42 pesticides and their metabolites in poultry eggs and productsby QuEChERS-UPLC-MS/MS

作　　者：吕青骎 王玮[1,2] 梁丽姣[3] 滕爽 徐幸莲[1,2] LV Qingqin;WANG Wei;LIANG Lijiao;TENG Shuang;XU Xinlian(Nanjing Agricultural University,College of Food Science and Technology,Nanjing 210095,China;National Center of Meat Quality and Safety Control/Supervision,Inspection and Testing Center for Quality of Meat-Products(Nanjing),Ministry of Agriculture,Nanjing Agricultural University,Nanjing 210095,China;Nanjing University of Finance and Economics,College of Food Science and Engineering,Nanjing 210095,China)

机构地区：[1]南京农业大学食品科技学院,江苏南京210095 [2]南京农业大学国家肉品质量安全控制工程技术研究中心,农业农村部肉及肉制品质量监督检验测试中心(南京),江苏南京210095 [3]南京财经大学食品科技与工程学院,江苏南京210095

出　　处：《食品与发酵工业》2020年第5期255-262,共8页Food and Fermentation Industries

基　　金：国家重点研发计划(2018YFC1602804);中央高校基本科研业务费专项资金资助(SYSB201815)。

摘　　要：利用QuEChERS(quick,easy,cheap,effective,rugged,safe)结合超高效液相色谱串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)建立同时检测禽蛋及其制品中42种农药及其代谢物残留的检测方法。以体积分数1%的乙酸乙腈为提取溶剂,加入NaCl除水后,经多功能针式过滤器至进样小瓶中,以体积分数为0.1%甲酸水溶液和5 mmol/L甲酸铵甲醇溶液作为流动相,采用UPLC-MS/MS方法检测。结果表明,各农药及代谢物在0.5~100μg/L范围内线性关系良好,相关系数大于0.9900,检出限为0.01~0.5μg/kg,样品加标回收率为74.13%~113.22%,相对标准偏差(relative standard deviation,RSD)为0.98%~14.29%(n=6)。建立的QuEChERS-UPLC-MS/MS方法可同时检测42种目标物,回收率好、精密度高、检出限低、且分析时间短,能够满足禽蛋及其制品中多种农药及其代谢物的同时检测。A method was established for the determination of 42 pesticides and their metabolites in eggs and products on the basis of QuEChERS(quick,easy,cheap,effective,rugged,safe)combined with ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The sample was extracted by acetonitrile(containing 1%acetic acid),dewatered by sodium chloride,and then uniformly passed through a multi-functional needle filter into the sampling vial.0.1%formic acid aqueous solution and 5 mmol/L ammonium formatting methanol solution were used as the mobile phase solution,and UPLC-MS/MS was used as a detection method.42 pesticides and their metabolites showed good linear in the range of 0.5-100μg/L,respectively,with the correlation coefficients above 0.9900.The limits of detection(LOD)were 0.01~0.5μg/kg,the recoveries of spiked samples were between 74.13%-113.22%and the relative standard deviations(RSD)were between 0.98%-14.29%(n=6).The QuEChERS-UPLC-MS/MS can detect 42 kinds of targets simultaneously with good reproducibility,high accuracy,low detection limit and short analysis time.The method could be widely used for simultaneous detection of pesticide residues in poultry eggs and products.

关 键 词：QUECHERS 超高效液相色谱串联质谱 农药残留 禽蛋 

分 类 号：TS253.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]