高效液相色谱-串联质谱法测定乳及乳制品中17种真菌毒素  

Determination of 17 Mycotoxins in Milk and Dairy Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：刘玲 叶沛 张巧艳[3] 申颖 董玉英[2] 蒋孟圆[4] 李文廷[2] LIU Ling;YE Pei;ZHANG Qiaoyan;SHEN Ying;DONG Yuying;JIANG Mengyuan;LI Wenting(School of Public Health,Kunming Medical University,Kunming 650500,China;Kunming Center for Disease Control and Prevention,Kunming 650228,China;Institute of Agro-Product Safety and Nutrition,Zhejiang Academy of Agricultural Sciences,Hangzhou 310021,China;Key Laboratory of Chemistry in Ethnic Medicinal Resources,State Ethnic Affairs Commission and Ministry of Education,Yunnan Minzu University,Kunming 650504,China)

机构地区：[1]昆明医科大学公共卫生学院,云南昆明650500 [2]昆明市疾病预防控制中心,云南昆明650228 [3]浙江省农业科学院农产品质量安全与营养研究所,浙江杭州310021 [4]云南民族大学民族药资源化学国家民委-教育部重点实验室,云南昆明650504

出　　处：《乳业科学与技术》2023年第5期18-26,共9页JOURNAL OF DAIRY SCIENCE AND TECHNOLOGY

基　　金：昆明市卫生科技人才培养项目(2022-SW(带头)-16);昆明市卫生科研课题项目(2022-12-06-001)。

摘　　要：基于高效液相色谱-串联质谱技术建立同时检测乳及乳制品中17种真菌毒素的方法。样品称量后加入定量同位素内标溶液,经20 mL乙腈-水-甲酸溶液(70∶29∶1,V/V)涡旋振荡提取,加入0.3 g氯化钠盐析,高速离心后上清液过0.22μm滤膜,用三重四极杆质谱在多反应监测模式下测定,通过同位素内标法定量。结果表明:在优化后的色谱及质谱条件下,17种真菌毒素线性范围良好,相关系数(r)均大于0.99,检出限为0.05~6.20μg/kg,定量限为0.2~20.0μg/kg,对低、中、高3个添加水平均具有良好的回收率和精密度,平均加标回收率为78.9%~119.5%,相对标准偏差为0.2%~8.4%。该方法操作便捷、稳定可靠、灵敏度高,能满足乳及乳制品中17种真菌毒素的定性定量分析要求,适用于实验室对乳及乳制品中17种真菌毒素的污染监测。To establish a method for simultaneous detection of 17 mycotoxins in milk and dairy products based on high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Samples(5.0000 g)were added to 20μL of a mixed solution of isotope-labeled internal standards,extracted with 20 mL of acetonitrile-water-formic acid solution(70:29:1,V/V)by vortex shaking,salted out with 0.3 g of sodium chloride,and then centrifuged at high speed.The supernatant was passed through a 0.22μm membrane filter,detected by triple quadrupole mass spectrometry in the multi-reaction detection mode and quantified by an internal standard method.Results:Under the optimized instrumental conditions,good linearity was observed for the 17 mycotoxins in the tested concentration ranges,with correlation coefficient(r)greater than 0.99.The limit of detection(LOD)was 0.05-6.20μg/kg,and the limit of quantitation(LOQ)was 0.2-20.0μg/kg.Good average recoveries(78.9%-119.5%)and precision(relative standard deviations(RSDs)0.2%–8.4%)were achieved at three spiked levels.The method is convenient,stable,reliable and sensitive,can meet the requirements of qualitative and quantitative analysis of the 17 mycotoxins in milk and dairy products,and is suitable for laboratory monitoring of the contamination of these mycotoxins in milk and dairy products.

关 键 词：乳及乳制品 真菌毒素 高效液相色谱-串联质谱 食品安全 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]