固相萃取/高效液相色谱-串联质谱法同时检测多类食品中二甲基黄、二乙基黄含量  

Determination of Dimethyl Yellow and Diethyl Yellow in Variety of Foods by Solid Phase Extraction/Liquid Chromatography-Tandem Mass Spectrometry

作　　者：赖国银[1] 伊雄海[2] 吴敏[1] 张志刚[1] 王传现[2] 徐敦明[1] 吕美玲[3] LAI Guo-yin YI Xiong-hai WU Min ZHANG Zhi-gang WANG Chuan-xian XU Dun-ruing LU Mei-ling(Technical Center of Xiamen Entry - Exit Inspection and Quarantine Bureau, Xiamen 361026, China Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China Agilent Technologies（China） Company Limited, Beijing 100102, China)

机构地区：[1]厦门出入境检验检疫局检验检疫技术中心,福建厦门361026 [2]上海出入境检验检疫局,上海200135 [3]安捷伦科技(中国)有限公司,北京100102

出　　处：《分析测试学报》2017年第3期393-397,共5页Journal of Instrumental Analysis

基　　金：福建省自然科学基金项目(2014J01057;2016J05045);国家质检总局科技计划项目(2016IK186);上海市技术标准专项(14DZ0501001;15DZ0503201)

摘　　要：建立了豆干、辣椒酱、豆腐乳、腐竹和饼干等样品中二甲基黄和二乙基黄残留量的液相色谱-串联质谱分析方法。基于二甲基黄和二乙基黄的化学结构特性,采用乙腈溶液提取。提取液酸化后经Bond Elut Plexa PCX阳离子交换树脂固相萃取净化,吹干复溶后,使用反相C_(18)色谱柱分离,电喷雾串联四极杆质谱正离子化多反应监测(MRM)模式检测。二甲基黄和二乙基黄的方法定量下限均为0.50μg/kg。对5种不同基质样品进行二甲基黄和二乙基黄0.50,5.0,80μg/kg 3个浓度水平的加标回收实验,得到二甲基黄和二乙基黄的平均回收率分别为76.4%~93.0%和76.1%~92.4%;相对标准偏差分别为1.7%~6.3%和1.9%~7.4%,可以满足食品中二甲基黄和二乙基黄快速筛查和定量分析的要求。A liquid chromatography-tandem mass spectrometric（LC-MS/MS） method was developed for the determination of dimethyl yellow and diethyl yellow in dried bean curd,chili sauce,tofuru,dried beancurd sticks and biscuit.In this study,based on the chemical structures of dimethyl yellow and diethyl yellow,the sample was first extracted using acetonitrile solution,and the extract was then acidified and purified with a Bond Elut Plexa PCX cation anion exchange cartridge.After drying and re dissolvation,the analytes were separated by reverse phase LC using a C18 column,followed by detection using triple quadrupole mass spectrometry with positive electrospray ionization in multiple reaction monitoring（MRM） mode.The limits of quantitation were both 0.50 μg/kg.The recoveries of dimethyl yellow and diethyl yellow in food samples at three spiked levels of 0.50,5.0,80 μg/kg were in the range of 76.1%-93.0% with relative standard deviations（RSDs） of 1.7%-7.4%.The method could meet the requirement for rapid screening and quantitative analysis of dimethyl yellow and diethyl yellow in foods.

关 键 词：二甲基黄 二乙基黄 固相萃取 液相色谱-串联质谱(LC-MS/MS) 

分 类 号：O657.63[理学—分析化学] TQ613.1[理学—化学]