[关键词]
[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,1.8 μm)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(r2>0.995),定量限均为50 μg/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。
[Key word]
[Abstract]
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,1.8 μm) 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 (r2 >0.995). The limits of quantitation (LOQs) were 50 μg/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.
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[基金项目]
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)