建立了一种基于超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法（UPLC-Q/Orbitrap HRMS）快速筛查及定量分析清咽类保健食品中12种非法添加药物的方法。样品经乙腈超声提取，高速离心，以ZORBAX XDB-C18（50 mm×2.1 mm，1.8 μm）为色谱柱，甲醇与0.1%甲酸水溶液（含5 mmol/L乙酸铵）为流动相，梯度洗脱，质谱采集用Q Extractive高分辨质谱中正离子扫描，一级全扫描和数据依赖的二级子离子扫描（Full MS/dd-MS2）监测模式，以Full MS提取高分辨母离子色谱峰的面积定量，以保留时间、一级母离子以及dd-MS2扫描所得的二级碎片离子信息建立数据库定性筛查。12种药物在7.63 min内的得到有效分离，精确质量数偏差不大于1.48×10-6，在1.00~200.00 µg/L范围内线性关系良好（相关系数≥0.999），测定下限为50.00~150.00 μg/kg，加标回收率在75.15%~117.65%之间，相对标准偏差（RSD）为0.89%~4.84%。该方法前处理简单、快速，分析检测准确，灵敏度高，选择性强，可用于清咽类保健食品中12种非法添加药物快速定性筛查和定量分析。

A method for rapid screening and quantitative analysis of 12 kinds of illegally added drugs in throat-cleaning healthcare food products based on ultra high performance liquid chromatography-quadrupole/elecrostatic orbitrap high resolution mass spectrometry (UPLC-Q/Orbitrap HRMS) was developed. The sample was extracted with acetonitrile and centrifuged at a high speed. The separation of the 12 target compounds was performed on a ZOBAX XDB-C18 column (50 mm × 2.1 mm, 1.8 μm) through a gradient elution with 0.1% formic acid (containing 5 mmol/L ammonium acetate) and methanol as the mobile phase. Mass spectrometry analysis was performed via the full MS/dd-MS2 acquisition with positive ionization mode, and the chromatographic peak areas obtained through extracting the accurate mass number of parent ions by full MS first-order mass spectrometry were quantified. A database was established for qualitative screening based on the retention time, primary precursor mass and secondary fragment ions information from DD-MS2 scans. The 12 kinds of drugs were effectively separated within 7.63 min with the mass accuracy deviation lower than 1.48×10-6. A good linearity was obtained in the range from 1.00 µg/L to 200.00 µg/L, with a correlation coefficients higher than 0.999. The lower limits of detection ranged from 50.00 µg/kg to 150.00 µg/kg. The average spiked recoveries for 12 target compounds were between 75.15% and 117.65%, with relative standard derivations (RSDs) ranged from 0.89% to 4.84%. The method was simple, fast, accurate, sensitive and selective, thus can be used for rapid qualitative screening and quantitative analysis of illegally added chemical drugs in throat-cleaning healthcare food products.

国家自然科学基金资助项目（21577042）；河南省市场监督管理局应用技术研究项目（2020sj36）