超高效液相色谱-静电场轨道阱高分辨质谱快速筛查保健品中23种非法添加西药成分  

Rapid Screening and Confirmation of 23 Illicit Western Medicine Components in Health Food Products by Ultra High Performance Liquid Chromatography-Orbitrap High Resolution Mass Spectrometry

作　　者：张晓光[1,2] 李强[1,2] 孙磊[1,2] 夏静[1,2] 张岩[1,2] 

机构地区：[1]河北省食品检验研究院,河北石家庄050091 [2]河北省食品安全重点实验室,河北石家庄050091

出　　处：《食品科学》2015年第14期187-191,共5页Food Science

基　　金：河北省科技条件建设项目(13965504D)

摘　　要：建立基于超高效液相色谱-四极杆-静电场轨道阱质谱的快速筛查和确证保健品中可能非法添加的23种降压类西药成分的方法。样品经过甲醇提取,用Acquity UPLC BEH C18柱（50 mm×2.1 mm,1.7μm）分离,以甲醇和体积分数0.1%甲酸溶液作为流动相进行梯度洗脱,采用正、负离子同时切换的扫描模式,在9 min内实现23种西药成分的检测。在全扫描模式下测定目标化合物的精确相对分子质量,与理论精确相对分子质量对比,相对质量偏差在0.2×10^-6-2.8×10^-6之间,有效地去除了基质干扰;建立了23种西药成分二级质谱数据库,实现对23种西药成分的定性筛查及同步定量。添加水平为0.2、0.5μg/kg和5.0μg/kg时,方法的回收率范围在72.3%-118.2%之间,相对标准偏差在0.5%-8.4%之间,检测限在0.2-0.5μg/kg之间。该方法可以作为降压功效保健品中非法添加的西药成分的高通量筛选和确认检测方法。A high performance liquid chromatography-linear ion trap/orbitrap high-resolution mass spectrometry（Orbitrap MS） method was developed for rapid screening and detection of 23 illicit western medicine components with antihypertensive efficacy in health foods. The samples were extracted with methanol, and the extracts were then separated on an Acquity UPLC BEH C18（50 mm×2.1 mm, 1.7 μm） using a binary solvent system composed of methanol and 0.1%formic acid in water by gradient elution. Both positive ion scan mode and negative ion scan mode were used to detect 23 western medicine components within 9 minutes. The relative molecular masses of the target compounds were obtained in full scan mode with a relative deviation in the range of 0.2×10^-6 to 2.8×10^-6 compared to the theoretical value, indicating effective elimination of the matrix interference. Tandem mass spectrometric database based on characteristic fragment ions for the 23 western medicines was built. This method allowed qualitative screening and quantitative analysis at the same time. Recoveries of the proposed method were in range of 72.3%–118.2% at spike levels of 0.2, 0.5 and 5.0 μg/kg with relative standard deviations（RSDs） between 0.5% and 8.4%, and the limits of detection were between 0.2 and 0.5 μg/kg. As a high-throughput and confirmatory method, it is useful for the determination of illicit western medicines as antihypertensive agents in health foods.

关 键 词：超高效液相色谱 静电场轨道阱高分辨质谱系统 降压类药物 保健品 

分 类 号：TS207.3[轻工技术与工程—食品科学]