Impurity profile study of repaglinide

Three unknown impurities and a byproduct in repaglinide bulk drug at levels below 0.1% (ranging from 0.05 to 0.1%) were detected by a simple isocratic reversed-phase high performance liquid chromatography (HPLC) method. These impurities were isolated from crude sample of repaglinide using reversed-p...

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Published inJournal of pharmaceutical and biomedical analysis Vol. 32; no. 3; pp. 461 - 467
Main Authors Krishna Reddy, K.V.S.R., Moses Babu, J., Mathad, Vijayavitthal T., Eswaraiah, S., Satyanarayana Reddy, M., Dubey, P.K., Vyas, K.
Format Journal Article
LanguageEnglish
Published Amsterdam Elsevier B.V 14.07.2003
Elsevier Science
Subjects
Analysis
Biological and medical sciences
Byproduct
Carbamates - analysis
Chromatography, High Pressure Liquid
Drug Contamination
General pharmacology
Hypoglycemic Agents - analysis
Identification and characterisation
Impurities
Magnetic Resonance Spectroscopy
Mass Spectrometry
Medical sciences
Pharmacology. Drug treatments
Piperidines - analysis
Repaglinide
Spectroscopy
Spectroscopy, Fourier Transform Infrared
Byproduct
Spectroscopy
Repaglinide
Impurities
Identification and characterisation
Drug
Impurity
HPLC chromatography
NMR spectrometry
Infrared spectrometry
Reversed phase chromatography
Qualitative analysis
Mass spectrometry
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Summary:Three unknown impurities and a byproduct in repaglinide bulk drug at levels below 0.1% (ranging from 0.05 to 0.1%) were detected by a simple isocratic reversed-phase high performance liquid chromatography (HPLC) method. These impurities were isolated from crude sample of repaglinide using reversed-phase preparative high performance liquid chromatography. Based on the spectroscopic data (IR, NMR and MS) the structures of these impurities (I, II and IV) and byproduct (III) were characterised as 4-carboxymethyl-2-ethoxy-benzoic acid (I), 4-cyclohexylaminocarbamoylmethyl-2-ethoxy-benzoic acid (II), 1-cyclohexyl-3-[3-methyl-1-(2-piperidin-1-yl-phenyl)-butyl]-urea (IV) and 1,3-dicyclohexyl urea (III), respectively. Their synthesis and formation is discussed.
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ISSN:0731-7085
1873-264X
DOI:10.1016/S0731-7085(03)00216-4