UPLC/Q-TOF-MS法检测2种中成药中土霉素、马来酸氯苯那敏和醋酸泼尼松

Detection of oxytetracycline,chlorpheniramine maleate and prednisone acetate in two Chinese traditional patent medicines by UPLC / Q-TOF-MS

目的建立UPLC/Q-TOF-MS法检测2种止咳平喘类中成药中非法添加的土霉素,马来酸氯苯那敏和醋酸泼尼松。方法咳喘王胶囊和清肺胶囊以甲醇提取;Agilent SB-C18色谱柱(2.1 mm×100 mm,1.8μm);流动相为甲醇-10 mmol/L醋酸铵溶液(含0.1%甲酸);离子源为ESI;正离子检测方式;利用保留时间、DAD紫外光谱图、一级质谱、二级质谱碎片信息等4方面信息并结合数据库进行定性、定量测定。结果 2批胶囊中均检测出以上3种非法添加成分。结论本方法专属性强、灵敏度高、操作简便,可用作止咳平喘类中成药的常规检测。

AIM To establish a method for detecting the contents of oxytetracycline,chlorpheniramine maleate and prednisone acetate illegally added in two Chinese traditional patent medicines for antitussive and antiasthmastics by UPLC / Q-TOF-MS. METHODS The analyses of Kechuanwang Capsules and Qingfei Capsules methanolic extracts were performed on Agilent SB-C18column（ 2. 1 mm × 100 m,1. 8 μm） with the mobile phase of methanol-0. 01 mol / L ammonium acetate（ containing 0. 1% formic acid） in a gradient elution manner. Electrospay ionization（ ESI） source was applied and operated in a positive ion mode,qualitative and quantitative data were measured by retention time,DAD spectrum,mass spectra and tandem mass spectra. RESULTS Three illegally added substances（ oxytetracycline,chlorpheniramine maleate and prednisone acetate） were all detected in two batches of capsules. CONCLUSION This method is specific,sensitive and easy to operate,which can be recommended as routine inspection.