QuEChERS EMR-Lipid净化结合超高效液相色谱-串联质谱法快速测定食品中非法添加工业染料  

Rapid Determination of Illegal Addition of Industrial Dyes in Foods by QuEChERS Using EMR-Lipid Sorbent Combined with Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：余晓琴 闵宇航 刘斯琪 李澍才 YU Xiaoqin;MIN Yuhang;LIU Siqi;LI Shucai(Sichuan Institute of Food Inspection,Chengdu 611731,China;Key Laboratory of Baijiu Supervising Technology for State Market Regulation,Chengdu 611731,China)

机构地区：[1]四川省食品检验研究院,四川成都611731 [2]国家市场监管重点实验室(白酒监管技术),四川成都611731

出　　处：《食品科学》2024年第16期268-283,共16页Food Science

基　　金：国家市场监督管理总局基金项目(2020-KYSB-008);四川省市场监督管理局科技计划项目(SCSJS2022005)。

摘　　要：建立采用增强型脂质去除净化填料(enhanced matrix removal lipid,EMR-Lipid)的QuEChERS净化技术结合超高效液相色谱-串联质谱同时测定食品中57种工业染料非法添加的快速分析方法。样品用乙腈提取,提取液经EMR-Lipid净化,采用Agilent ZORBAX Eclipse RRHD C18色谱柱(3.0 mm×150 mm,1.8μm)分离、流动相采用乙腈和体积分数0.1%甲酸溶液进行梯度洗脱、电喷雾电离源正离子模式扫描、多反应监测模式检测、外标法定量。结果表明:57种工业染料在20~300 ng/mL质量浓度内线性关系良好,相关系数r>0.999;方法检出限为10μg/kg、定量限为25μg/kg;在25、100、250μg/kg加标水平下的回收率为72.1%~119.1%,相对标准偏差(n=6)为0.19%~4.58%;采用该方法检测豆制品、调味品、水产品、肉制品各20批次中的工业染料,在1批次花椒粉中检出碱性嫩黄,检出量为32.9μg/kg。所建方法具有快速、准确、灵敏的优点,适用于食品中57种工业染料非法添加的快速测定。An analytical method based on quick,easy,cheap,effective,rugged and safe(QuEChERS)cleanup using an enhanced matrix removal lipid(EMR-Lipid)sorbent combined with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established for the rapid determination of 57 industrial dyes illegally added in foods.The sample was extracted with acetonitrile,and the extract was purified by QuEChERS.The analytes were separated on an Agilent ZORBAX Eclipse RRHD C18 column(3.0 mm×150 mm,1.8μm)with gradient elution using a mobile phase composed of acetonitrile and 0.1%formic acid,detected using an electrospray ionization source operated under the positive mode with multiple reaction monitoring(MRM),and quantified by an external standard method.The results showed that good linearity was observed for all analytes in the concentration range from 20 to 300 ng/mL with correlation coefficients higher than 0.999.The limits of detection(LOD)and quantitation(LOQ)were 10 and 25μg/kg,respectively.The recoveries at 3 spiked levels(25,100 and 250μg/kg)were 72.1%–119.1%,with relative standard deviations(RSDs,n=6)of 0.19%–4.58%.The developed method was used to detect illegal addition of industrial dyes in soybean products,condiments,aquatic products,and meat products(n=20 for each type).Alkaline yellow was detected in one bath of Sichuan pepper powder at a level of 32.9μg/kg.In conclusion,this method is rapid,accurate,sensitive,and suitable for the determination of the 57 industrial dyes illegally added in foods.

关 键 词：增强型脂质去除净化填料 超高效液相色谱-串联质谱 工业染料 食品 

分 类 号：O657.63[理学—分析化学]