UPLC-MS/MS法快速检测减肥类保健食品中5种非法添加化学成分

摘要

Objective The study aimed to develop a specific, sensitive and rapid UPLC-MS/MS method to identify 5 illegal additives in slimming health food.MethodsThe ultra performance liquid chromatography-electrospray ion trap mass spectrometry method was used to detect the samples extracted by methanol. The separation was performed on Waters UPLC using BEH-C18 column with a gradient elution. The mobile phase was consisted of 20mmol/L ammonium acetate (containing 0.1% acetic acid) and methanol. Qualitative and quantitative analysis of caffeine, furosemide, fenfluramine, phenolphthalein and sibutramine was conducted in the MRM mode by UPLC-MS/MS.ResultsA good resolution of 5 chemical drugs within 6 min was obtained by UPLC-MS/MS. The calibration curves showed good linear relationship in the range of 1-200ng/mL for each component. The determination limits was at 0.0025-0.0075mg/g, and the average recovery rate was 97.7%-100.7%. Conclusion The method was proved to be specific, rapid and sensitive, which was able to be used to identify 5 illegal additives in weight reducing health food.%目的：建立专属、灵敏的UPLC-MS/MS方法用于快速定性定量检测减肥类保健食品中5种非法添加化学成分。方法供试样品经甲醇提取后，采用超高效液相色谱-串联质谱法（UPLC-MS/MS），以BEH-C18为分析柱，流动相采用含0.1%冰醋酸的20mmol/L醋酸铵水溶液和甲醇进行梯度洗脱，电喷雾电离（ESI）、多重反应监测（MRM）扫描模式，对保健食品中非法添加的盐酸西布曲明、酚酞、盐酸芬氟拉明、咖啡因、呋塞米等5种化学成分进行快速定性定量检测。结果所建立方法能快速定性定量检测保健食品中5种非法添加化学药物成分，5种成分在6min内完全分离，且线性良好，平均加样回收率在97.7%～100.7%，方法检出限为0.0025～0.0075mg/g。结论所建方法快速、灵敏、专属性强，适用于减肥类保健食品中非法添加化学成分的快速定性定量检测。