轨道离子阱快速筛查及定量分析保健食品中73种非法添加成分

Rapid screening and quantitative analysis of 73 kinds of chemicals illegally added in the healthy foods by Orbitrap mass spectrometry

基于超高效液相色谱—静电场轨道阱高分辨质谱建立了保健食品中73种非法添加成分的高通量定性筛查和定量分析方法。样品经甲醇溶液进行超声提取,以水(含0.1%甲酸)和乙腈溶液为流动相,采用Waters Acquity UPLC HSS T3色谱柱(100 mm×2.1 mm, 1.8 μm)进行梯度洗脱,利用加热电喷雾电离源(HESI)进行正负离子同时切换扫描,采用全扫描/数据依赖二级质谱(Full-scan ddMS 2 )模式采集数据,通过Trace Finder软件利用自建数据库进行定性分析,以母离子峰面积进行定量分析,实现73种西药成分的定性筛查及同步定量。试验结果表明,各药物检出限为2~20 μg/kg,定量限为6~60 μg/kg,添加水平为100,200,1 000 μg/kg时,方法的回收率在72.2%~117.5%,相对标准偏差为2.3%~ 6.8%。在一定线性范围内,各药物的线性相关系数均大于0.99。该方法可以作为保健食品中非法添加西药成分的高通量定性筛查和定量检测方法。

A high-throughput qualitative screening and quantita-tive method of ultra-high performance liquid chromatography combined with orbitrap mass spectrometry(UPLC-Orbitrap-MS) was developed to determine 73 kinds of chemicals illegally added in the healthy foods. The samples were extracted with methanol using ultrasonic extraction. The separation was eluted by gradient on a Waters Acquity UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm), with a mobile phase consisting of water (0.1% formic acid) and acetonitrile in both positive and negative mode. The data were acquired via full-scan data-dependent MS/MS (full scan-ddMS 2 ). The qualitative analyses of the compounds were performed through the database established by Trace Finder software, and the quantitative detection were undertaken through the area of precursor ions. The results showed that each target had good linearity in its own concentration range, and the correlation coefficients were higher than 0.99. The limits of determination (LODs) were between 2~20 μg/kg, and the limits of quantification (LOQs) were between 6~60 μg/kg. The recoveries of the proposed method were in range of 72.2%~117.5% at spiked levels of 100, 200, and 1 000 μg/kg with deviations (RSDs) between 2.3%~ 6.8%. It could be concluded that the high-throughput, qualitative and quantitative method reported in this study was useful for the determination of illicit drugs in functional foods.