title: Isolation and characterization of benazepril unknown impurity by chromatographic and spectroscopic methods.
abstract: The presence of unknown impurity of the order of 0.2% was identified in benazepril using liquid chromatographic technique employing binary gradient system comprising acetic acid and ammonia in water and acetonitrile as the mobile phase. LCMS data corresponds to hydroxylated benazepril (OHB) derivative possessing the molecular formula C(24)H(28)N(2)O(6). This impurity was isolated using isocratic system containing ammonium acetate and acetonitrile and the product was characterized using FT-IR, (1)H and (13)C NMR and mass spectroscopy to ascertain the structure of the impurity. The spectroscopic analysis revealed the presence of hydroxyl function on C(17) carbon atom of benazepril molecule. The plausible mechanism for the formation of OHB species is proposed.
authors.affiliation: Lupin Research Park, Survey No. 46A/47A, Nande Village, Pune 411042, India.
authors.forename: Vikas R
authors.initials: VR
authors.lastname: Shinde
authors.forename: Anurag
authors.initials: A
authors.lastname: Trivedi
authors.forename: P R
authors.initials: PR
authors.lastname: Upadhayay
authors.forename: N L
authors.initials: NL
authors.lastname: Gupta
authors.forename: D G
authors.initials: DG
authors.lastname: Kanase
authors.forename: Rajeev C
authors.initials: RC
authors.lastname: Chikate
mesh_terms: D001552:Benzazepines / Q000032:analysis*; D002853:Chromatography, Liquid; D004340:Drug Contamination; D009682:Magnetic Resonance Spectroscopy; D013058:Mass Spectrometry; D017550:Spectroscopy, Fourier Transform Infrared
chemical_list: D001552:Benzazepines; C044946:benazepril