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机构地区:[1]江苏省无锡药品检验所,江苏无锡214028 [2]江南大学药学院,江苏无锡214122
出 处:《中国现代应用药学》2016年第9期1160-1165,共6页Chinese Journal of Modern Applied Pharmacy
摘 要: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 a method for rapidly qualitative and quantitative detection of phenformin hydrochloride, glibenclamide and pioglitazone hydrochloride illegally added in traditional Chinese medicines for antidiabetics by UPLC-Q-TOF-MS. METHODS The Aglient ZORBAX SB C18(2.1 mm×100 mm, 1. 8 μm) column was used, with the mobile phase of methanol-10 mmol·L^-1 ammonium acetate(0.1% formic acid) by gradient elution. Electrospay ionization(ESI) source was applied and operated in the positive ion mode. Qualitative and quantitative detection were analysized by retention time, DAD, mass spectra, and tandem mass spectra as four aspects information. RESULTS Phenformin hydrochloride, glibenclamide and pioglitazone hydrochloride were all detected illegally added in five batches capsules. CONCLUSION This method is specific, sensitive, easy to operate and can be used to detect the phenformin hydrochloride, glibenclamide and pioglitazone hydrochloride illegally added in traditional Chinese medicinal preparation for antidiabetics.
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