采用液相色谱、核磁共振和质谱法对潜在降血糖剂 G004 中的杂质进行定性和定量研究。
Qualitative and quantitative studies on impurities in G004, a potential hypoglycaemic agent, using liquid chromatography, nuclear magnetic resonance and mass spectrometry.
机构信息
Department of Pharmaceutical Analysis, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China.
出版信息
J Pharm Biomed Anal. 2011 Nov 1;56(3):627-32. doi: 10.1016/j.jpba.2011.06.017. Epub 2011 Jun 28.
G004, 1-(4-(2-(4-bromobenzenesulphonamino) ethyl) phenylsuphonyl)-3-(trans-4-methylcyclohexyl) urea, is being developed as a potential hypoglycaemic agent. In this study, the related compounds in the bulk drug substance of G004 were analyzed both qualitatively and quantitatively. An unknown compound in the drug, which has never been reported, was isolated using preparative liquid chromatography and characterized as 1-(4-(2-(2-bromobenzenesulphonamino) ethyl) phenylsuphonyl)-3-(trans-4-methylcyclohexyl) urea using nuclear magnetic resonance and mass spectrometry. Moreover, a reversed-phase liquid chromatography method was developed for quantification of both the major impurities and the main constituent. The proposed method was validated and applied during impurity studies and quality control analysis of the bulk drug and laboratory-prepared samples of G004.
G004，1-(4-(2-(4-溴苯磺酰胺基)乙基)苯磺酰基)-3-(反式-4-甲基环己基)脲，正在被开发为一种有潜力的降血糖药物。在这项研究中，对 G004 原料药中的相关化合物进行了定性和定量分析。使用制备液相色谱法分离出药物中的一种未知化合物，该化合物从未有过报道，通过核磁共振和质谱鉴定为 1-(4-(2-(2-溴苯磺酰胺基)乙基)苯磺酰基)-3-(反式-4-甲基环己基)脲。此外，还开发了一种反相液相色谱法来定量测定主要杂质和主成分。所提出的方法经过验证，并应用于原料药和实验室制备的 G004 样品的杂质研究和质量控制分析。
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