UPLC-IT/TOF MS快速筛查确证保健食品中36种非法添加的减肥、降血脂、通便类药物

Fast screening and identification of 36 illegally added weight-loss,lipidlowering, cathartic drugs in health products by UPLC-IT/TOF MS

目的基于超高效液相色谱-离子阱/飞行时间质谱(UPLC-IT/TOF MS)建立保健食品中36种非法添加的减肥、降血脂、通便类药物的快速筛查和确证方法。方法样品采用甲醇超声提取,Waters BEH Shield RP18色谱柱(100 mm×2.1 mm,1.7μm)分离,用含0.1%甲酸的10 mmol·L^-1乙酸铵水溶液和甲醇进行梯度洗脱,正、负离子电喷雾离子化扫描模式扫描一级质谱(MS^1)、二级质谱(MS^2)、三级质谱(MS^3)。利用保留时间和一级母离子的精确质量数快速筛查目标化合物,利用二级质谱和三级质谱的碎片离子进一步确证。结果 36种药物检出限(LOD)为0.02~38 mg·L^-1,回收率为70%~120%,相对标准偏差小于10%。应用本法测定74批样品,检出酚酞、西布曲明、N-单去甲基西布曲明,N,N-双去甲基西布曲明、氟西汀、咖啡因等非法添加药物。结论本方法具有准确、简便、快速的特点,可用于减肥类、降血脂类和通便类保健食品中36种非法添加药物的快速筛查和确证。

Objective To simultaneous determine 36 illegally added weight-loss, lipid-lowering, cathartic drugs in health products by ultra performance liquid chromatography-ion trap/time of flight high resolution mass spectrometry(UPLC-IT/TOF MS). Methods The target compounds were extracted with methanol by sonication extraction. The extracts were separated by Waters BEH Shield RP18 column(100 mm×2.1 mm, 1.7 μm) with gradient elution. Ammonium acetate(10 mmol·L^-1) containing 0.1%(v/v) formic acid and methanol were used as the mobile phase, and were finally analyzed by UPLC-IT/TOF MS in both positive and negative ESI modes. Results The accurate mass of parent ion and retention time in MS1 spectrum were used to fast screen 36 illegally added weight-loss, lipid-lowering, cathartic drugs and further confirmed by fragments of MS2 and MS3 spectrum. The LODs of each target were 0.02-38 mg·L^-1. The average recoveries of these targets at 3 spiked levels were 70%^-120%, and the relative standard deviations(n = 6) were less than 10%. This method was used to determine phenolphthalein, sibutramine hydrochloride, N-demethylatedsibutramine hydrochloride, N, N-didesmethylsibutramine hydrochloride, fluoxetine, caffeine and other illegally added drugs in 74 batches of samples. Conclusion The method is rapid, simple and accurate, and can be used for the rapid screening and confirmation of 36 illegally added weight-loss, lipid-lowering, cathartic drugs in health products.