Orbitrap高分辨质谱用于保健食品中15种非法添加减肥类药物的筛查鉴定

建立了筛查保健食品中非法添加的15种减肥类化合物的液相色谱-Orbitrap高分辨质谱联用法和TraceFinder筛查数据库。样品以甲醇为提取溶剂,上清液过滤后直接进行液相色谱-质谱联用分析。质谱采用Full MS/dd-MS 2扫描模式,正负离子同时检测。将采集的数据文件导入TraceFinder筛查软件,利用软件构建了化合物数据库及筛查方法进行快速、自动、高精度筛查,确定样品中是否违法添加了减肥类药物,并对阳性样品进行定量分析。方法学验证结果表明,所有化合物均显示出优异的线性关系,标准曲线回归系数( r )均大于0.998,回收率范围为79.7%~95.4%,精密度在3.3%~8.7%之间。应用该方法对29批保健食品进行了测定,在6批阳性样品中检出了4种化合物。该方法可实现自动、高精度筛查鉴定,为打击非法添加提供了新的手段。

Application of Orbitrap high resolution mass spectrometry for the screening and identification of 15 adulterated weight loss compounds in dietary supplements

A liquid chromatography-Orbitrap high resolution mass spectrometry (LC-HRMS) method and a TraceFinder database were developed for the screening and identification of 15 adulterated weight loss compounds in dietary supplements. The samples were extracted with methanol and filtered through a 0.22 μm microfiltration membrane prior to LC-HRMS analysis. The Full MS/dd-MS² mode was utilized in both positive and negative ion modes and the collected data were imported into the TraceFinder screening software. The established compound database and screening method were used for rapid, automatic, and high-precision screening to determine if the weight loss compounds were adulterated. The method validation results indicated that all of the analytes showed excellent linear relationships with regression coefficients (r) above 0.998. The recoveries were in the range of 79.7%-95.4% while the precisions ranged from 3.3% to 8.7%. The method and database were used to screen weight loss adulterants in 29 batches of dietary supplements; six batches of samples tested positive for adulterants with the identification of four compounds including sibutramine. This method enables the automatic high-precision screening and identification of adulterants, providing a novel and powerful tool for combating the increasingly rampant occurrence of adulteration in dietary supplements.