title: Qualitative and quantitative studies on impurities in G004, a potential hypoglycaemic agent, using liquid chromatography, nuclear magnetic resonance and mass spectrometry.
abstract: 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.
authors.affiliation: Department of Pharmaceutical Analysis, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China.
authors.forename: Wenyuan
authors.initials: W
authors.lastname: Liu
authors.forename: Ainan
authors.initials: A
authors.lastname: Zhou
authors.forename: Feng
authors.initials: F
authors.lastname: Feng
authors.forename: Huibin
authors.initials: H
authors.lastname: Zhang
authors.forename: Jinpei
authors.initials: J
authors.lastname: Zhou
authors.forename: Wenlong
authors.initials: W
authors.lastname: Huang
mesh_terms: D056148:Chromatography, Reverse-Phase / Q000379:methods; D004340:Drug Contamination; D007004:Hypoglycemic Agents / Q000032:analysis* / Q000737:chemistry*; D009682:Magnetic Resonance Spectroscopy / Q000379:methods; D013058:Mass Spectrometry / Q000379:methods; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013438:Sulfhydryl Compounds / Q000032:analysis* / Q000737:chemistry*; D014508:Urea / Q000031:analogs & derivatives* / Q000032:analysis / Q000737:chemistry
chemical_list: C547418:1-(4-(2-(4-bromobenzenesulfonamino) ethyl) phenylsulfonyl)-3-(trans-4-methylcyclohexyl)urea; D007004:Hypoglycemic Agents; D013438:Sulfhydryl Compounds; D014508:Urea