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目的建立专属、灵敏的HPLC-MS/MS方法甄别中药制剂及保健食品中可能添加的氯噻嗪、盐酸西布曲明、酚酞、吲哒帕胺、布美他尼、吉非罗齐等6种化学减肥药物。方法样品经甲醇提取,采用液相色谱-离子阱质谱联用法测定。色谱条件:Inertsil ODS-3色谱柱(4.6mm×250mm,5μm),梯度洗脱:流动相A为0.1%醋酸溶液;流动相B为乙腈,质谱条件:离子源ESI,选择正负离子全扫描、选择离子监测(SIM)、多反应监测(MRM)方式检测临床常用的6种化学减肥药物,研究了这6种药物的质谱裂解规律。通过比较样品峰与对照品峰的相对分子质量、二级质谱碎片信息和液相色谱保留时间,确定样品中是否违法添加了化学药物。结果应用本法检测了12批市售减肥类中药制剂及保健食品,其中1种减肥保健食品中检出西布曲明及酚酞,1种减肥保健食品中检出西布曲明,另外2种减肥保健食品检出酚酞。结论该法简便、快捷,灵敏度高、专属性强,可作为检测中药制剂及保健食品中非法掺入减肥类化学药的有效手段。
OBJECTIVE To establish a sensitive and sensitive HPLC-MS / MS method for the determination of chlorothiazide, sibutramine hydrochloride, phenolphthalein, indapamide, bumetanide and gemfibrozil in traditional Chinese medicine and health food Chemical weight loss drugs. Methods The samples were extracted with methanol and determined by liquid chromatography-ion trap mass spectrometry. Chromatographic conditions: Inertsil ODS-3 column (4.6mm × 250mm, 5μm), gradient elution: mobile phase A 0.1% acetic acid solution; mobile phase B acetonitrile, mass spectrometry conditions: ion source ESI, Selected ion monitoring (SIM) and multi-reaction monitoring (MRM) were used to detect six kinds of chemical weight-loss drugs commonly used clinically, and the mass spectrometry lysis patterns of these six drugs were studied. By comparing the molecular mass of the sample peak with that of the reference peak, secondary MS fragment information, and LC retention time, determine whether the sample was illegally added with a chemical. Results The method was applied to detect 12 batches of TCM slimming preparations and health food products. Among them, sibutramine and phenolphthalein were detected in 1 weight loss health food, sibutramine was detected in 1 weight loss health food, and the other 2 Weight loss health food detection phenolphthalein. Conclusion The method is simple, rapid, sensitive and specific. It can be used as an effective measure to illegally incorporate slimming chemicals in traditional Chinese medicine and health food.