论文部分内容阅读
目的建立UPLC Q-TOF MS快速检测降糖类中成药中非法添加的盐酸苯乙双胍、格列本脲、盐酸吡格列酮。方法采用Aglient ZORBAX SB C18色谱柱(2.1 mm×100 mm,1.8μm),甲醇-10 mmol·L?1醋酸铵溶液(含0.1%甲酸)为流动相,梯度洗脱;离子源为ESI,正离子检测方式;利用保留时间、DAD紫外光谱图、一级质谱和二级质谱碎片信息四方面信息并结合数据库,对10种降糖类化学成分进行质谱定性,同时对5批降糖类中成药中非法添加的盐酸苯乙双胍、格列本脲、盐酸吡格列酮进行定性、定量测定,并对这3种化学物质的裂解规律进行初步解析。结果 5批胶囊中均检测出盐酸苯乙双胍、格列本脲、盐酸吡格列酮3种成分。结论本方法专属性强、灵敏度高、操作简便,可用作降糖类中成药中非法添加盐酸苯乙双胍、格列本脲、盐酸吡格列酮的检测。
OBJECTIVE To establish UPLC Q-TOF MS for rapid detection of phenformin hydrochloride, glibenclamide and pioglitazone illegally added in hypoglycemic proprietary Chinese medicines. Methods Aglient ZORBAX SB C18 column (2.1 mm × 100 mm, 1.8 μm) and methanol-10 mmol·L-1 ammonium acetate solution (containing 0.1% formic acid) were used as the mobile phase and gradient elution. The ion source was ESI. Ion detection methods; using retention time, DAD UV spectra, MS and MS two fragments of information and four databases, the chemical composition of 10 kinds of hypoglycemic mass spectrometry qualitative analysis of five batches of hypoglycemic Chinese patent medicine Illegally added phenformin hydrochloride, glyburide and pioglitazone hydrochloride were determined qualitatively and quantitatively, and the cleavage regularities of the three chemical substances were preliminarily analyzed. Results Three batches of capsules were detected phenformin hydrochloride, glyburide, pioglitazone hydrochloride three kinds of ingredients. Conclusion This method is highly specific, sensitive and easy to operate. It can be used as a detection method of illegally added phenformin hydrochloride, glibenclamide and pioglitazone hydrochloride in Chinese traditional medicine.