UPLC-MS/MS测定凉果类酵素食品中的致泻类非法添加物  

Determination of illegal laxative additives in cold fruit enzymes by UPLC-MS/MS

作　　者：裘一婧 贾彦博[1] 江海[1] 孙岚 陈美春[1] 陈丽芳 余菁 林舒忆 QIU Yijing;JIA Yanbo;JIANG Hai;SUN Lan;CHEN Meichun;CHEN Lifang;YU Jing;LIN Shuyi(Hangzhou Institute for Food and Drug Control,Hangzhou 310022,China)

机构地区：[1]杭州市食品药品检验研究院,浙江杭州310022

出　　处：《发酵科技通讯》2024年第1期1-7,共7页Bulletin of Fermentation Science and Technology

基　　金：浙江省市场监督管理局科研计划项目(20200319)。

摘　　要：建立了一种简便准确检测凉果类酵素食品中非法添加多种致泻类化合物的UPLC-MS/MS检测方法。采用超微冷冻技术粉碎样本,用Oasis PRIME HLB固相萃取SPE净化;采用UPLC-MS/MS法,以浓度为0.02 mol/L的乙酸铵水溶液甲醇为流动相梯度洗脱,以CORTECS UPLC C18(1.6μm,2.1 mm×100 mm)色谱柱进行分离;采用串联四级杆质谱仪对凉果类酵素食品中的6种致泻类非法添加化合物进行定量检测。检测结果:线性范围为1~1000μg/L,相关性r^(2)≥0.9961;方法检测限LOD为0.1~1.0μg/kg,定量限LOQ为0.3~3.0μg/kg,高、中、低平均回收率均为82.5%~105.3%;日内精密度的RSD(n=9)为0.8%~3.7%。该检测方法专属性强、操作快捷,可作为凉果类酵素食品中致泻类非法添加化合物的有效检测方法。A simple and accurate detection method for multiple illegal laxative additives in cooling fruit enzyme products has been established using UPLC-MS/MS.Sample pulverization was achieved through ultra-micro cryogenic technology,followed by purification using Oasis PRIME HLB solid-phase extraction(SPE).The UPLC-MS/MS method employed a gradient elution with a mobile phase consisting of a 0.02 mol/L ammonium acetate aqueous solution and methanol.Separation was carried out using a CORTECS UPLC C18(1.6μm,2.1 mm×100 mm)chromatographic column.Quantitative detection of six illegal laxative additives in cooling fruit enzyme products was conducted using a tandem quadrupole mass spectrometer.Results:the linear range was 1~1000μg/L,correlation r ^(2)≥0.9961;the detection limits of LOD were 0.1~1.0μg/kg,the limits of quantification of LOQ were 0.3~3.0μg/kg,and the average recoveries were 82.5%~105.3%.Intraday precision RSD(n=9)ranged from 0.8%to 3.7%.The method has strong specificity and fast operation,and can be used as an effective method for the detection of compounds causing illegal laxative additives in cold fruit enzymes.

关 键 词：UPLC-MS/MS 凉果类 酵素食品 添加物 

分 类 号：O657.63[理学—分析化学]