新型脱脂前处理净化-UPLC-MS/MS法测定食用油中6种真菌毒素  

Simultaneous Determination of 6 Kinds of Mycotoxin in Oil by Enhanced Matrix Removal-Lipid-High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：孔芳 闻胜[1] 刘小红[1] 杨荣娇 罗苹[1] 唐琳[1] 李永刚[1] KONG Fang;WEN Sheng;LIU Xiaohong;YANG Rongjiao;LUO Ping;TANG Lin;LI Yonggang(Hubei Provincial Key Laboratory for Applied Toxicology,Hubei Provincial Centre for Disease Control and Prevention,Wuhan 430079,China)

机构地区：[1]湖北省疾病预防控制中心,应用毒理湖北省重点实验室,湖北武汉430079

出　　处：《食品科技》2023年第5期293-299,共7页Food Science and Technology

基　　金：湖北省卫生健康委2021—2022年度面上项目(WJ2021M209);2022年武汉市预防医学科研专项重点项目(WY22A02)。

摘　　要：研究建立了一种采用新型脱脂前处理(EMR-Lipid)净化技术-高效液相色谱-串联质谱法同时测定食用油中黄曲霉毒素(AFB_(1)、AFB_(2)、AFG_(1)、AFG_(2))、赭曲霉毒素A(OTA)和玉米赤霉烯酮(ZEN)的方法。样品用含1%的乙酸乙腈溶液提取,通过EMR-Lipid净化剂净化后,以C_(18)色谱柱分离,用乙腈:甲醇(1:1)-5 mmol/L乙酸铵溶液进行梯度洗脱,采用高效液相色谱-串联质谱法测定,多反应监测(MRM)模式和同位素内标法定量。6种真菌毒素在一定质量浓度范围内线性良好,相关系数大于0.99,检出限为0.04~0.40μg/kg,定量限为0.12~1.20μg/kg,平均回收率为91.2%~119.8%,相对标准偏差(RSD)为2.9%~9.1%。该方法简单快速、灵敏可靠,适用于食用油中6种真菌毒素的快速准确检测。To develop a method for the simultaneous determination of aflatoxin(AFB_1,AFB_2,AFG_1,AFG_2),ochratoxin A(OTA) and zearalanone(ZEN) in edible oil by enhanced matrix removal-lipid(EMR-Lipid)-high performance liquid chromatography-tandem mass spectrometry.The oil sample was extracted with 1% acetic acid-acetonitrile solution,purified by EMR-Lipid sorbent,separated by C_(18) chromatographic column with acetonitrile:methanol(1:1)-5 mmol/L ammonium acetate as mobile phase,the analyte was determined by high performance liquid chromatography-tandem mass spectrometry,and quantified by multiple reaction monitoring mode with internal standard method.The method had good linear relationship in the range of certain mass concentrations with correlation coefficients above 0.99,the limits of detection were 0.04-0.40 μg/kg,and the limits of quantitation were and 0.12-1.20 μg/kg,the recoveries and the relative standard deviations were in the range of 91.2%-119.8% and 2.9%-9.1%.This method is simple and fast,stable and reliable,and suitable for the simultaneous determination of 6 kinds of mycotoxin in oil.

关 键 词：新型脱脂前处理净化 高效液相色谱-串联质谱法 食用油 真菌毒素 

分 类 号：TS207.4[轻工技术与工程—食品科学]