高分辨质谱法快速筛查和定量分析改善胃肠道功能类保健食品中的22种非法添加化合物  

Rapid Screening and Quantitative Analysis of 22 Illegally Added Compounds in Gut Health-improving Foods by High-resolution Mass Spectrometry

作　　者：袁阳蕾 袁利杰 郭立净 石璐 YUAN Yanglei;YUAN Lijie;GUO Lijing;SHI Lu(Henan Institute of Food Inspection,Key Laboratory of Food Safety Quick Testing and Smart Supervision Technology for State Market Regulation,Henan Special Food Engineering Technology Center,Zhengzhou 450003,China)

机构地区：[1]河南省食品检验研究院,国家市场监管重点实验室(食品安全快速检测与智慧监管技术),河南省特殊食品工程技术研究中心,河南郑州450003

出　　处：《现代食品科技》2023年第1期311-319,共9页Modern Food Science and Technology

基　　金：国家自然科学基金资助项目(21577042);河南省市场监督管理局科技计划项目(2020sj36)。

摘　　要：建立一种超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法,快速筛查同时定量分析保健食品中22种非法添加化合物。该研究以市面上常见的改善胃肠道功能类保健食品(片剂和口服液基质)为研究对象,样品经甲醇涡旋振荡和超声提取;用Agilent ZORBAX Eclipse XDB-C18(2.1 mm×50 mm,1.8μm)色谱柱分离,φ=0.1%甲酸水和甲醇梯度洗脱;质谱条件采用正离子扫描,Full MS/dd-MS2(一级全扫描/数据依赖的二级扫描)模式,以化合物的保留时间、一级母离子和自动触发采集的二级碎片离子信息建立数据库,进行高通量定性筛查,以一级母离子进行定量分析,22种化合物在6.5 min内得到有效分离,精确质量数偏差≤1.77×10^(-6)。结果表明,各目标化合物在5~500 ng/mL的浓度范围内线性关系良好(r^(2)>0.995),定量限均为50μg/kg,片剂回收率为82.11%~116.16%,口服液回收率为83.64%~117.21%。该方法操作简单快速,灵敏度高,结果准确,适用于片剂和口服液基质的改善胃肠道功能类保健食品中22种非法添加化合物的快速筛查和定量分析。A method for rapid screening and quantitative analysis of 22 kinds of illegally added compounds in health-promoting foods using ultra-performance liquid chromatography-quadrupole/electrostatic orbitrap high-resolution mass spectrometry was established.In this paper,the commonly marketed gut function-improving healthcare products(tablets and oral liquid matrices)were taken as the research objects.Samples were extracted with methanol by vortex oscillation and ultrasonic treatment,and separated on an Agilent ZORBAX Eclipse XDB-C18 column(2.1 mm×50 mm,1.8μm)using 0.1%formic acid aqueous solution and methyl alcohole as the mobile phase for gradient elution.Mass spectrometry analyses adopted a positive ion scan and full MS/dd-MS2 mode,and a database was established based on the retention times of compounds,primary parent ions and secondary fragment ions information collected automatically for high-throughput qualitative screening and quantitative analyses with primary parent ions.The 22 kinds of chemical compounds were well separated within 6.5 minutes with the mass accuracy deviation less than 1.77×10^(-6).The results showed a good linear relationship for each target compound in the concentration range of 5 ng/mL~500 ng/mL(r^(2)>0.995).The limits of quantitation(LOQs)were 50μg/kg.The recoveries were 82.11%~116.16%for tablet samples and 83.64%~117.21%for the oral liquid samples.This method is simple,rapid,sensitive and accurate,thus suitable for rapid screening and quantitative analysis of 22 kinds of illegally added compounds in gut function-improving healthcare products in tablet and oral liquid forms.

关 键 词：改善胃肠道功能 保健食品 非法添加 高效液相色谱-四极杆/静电场轨道阱高分辨质谱 

分 类 号：O657.63[理学—分析化学] TS218[理学—化学]