LC and LC–MS/MS studies for the identification and characterization of degradation products of acebutalol

Publication date: Available online 15 March 2018Source: Journal of Pharmaceutical AnalysisAuthor(s): Uday Rakibe, Ravi Tiwari, Anand Mahajan, Vipul Rane, Pravin WakteAbstractThe aim of the present investigation was to demonstrate an approach involving use of liquid chromatography (LC) and liquid chromatography-mass spectrometry (LC-MS) analytical techniques to separate, identify and characterize very small quantities of degradation products (DPs) of acebutolol without their isolation from the reaction mixtures. The drug was subjected to oxidative, hydrolytic, thermal and photolytic stress conditions as per International Conference on Harmonization (ICH) guideline Q1A(R2). Among all the stress conditions the drug was found to be labile in hydrolytic (acidic & basic) and photolytic stress conditions, while it was stable to water induced hydrolysis, oxidative and thermal stress conditions. A total of four degradation products were formed. A C18 column employed for the separation of all the DPs on a gradient mode by using high-performance liquid chromatography (HPLC). All the DPs were characterized with the help of their fragmentation pattern and the masses obtained upon LC-MS/MS and MSn analysis. All the hitherto unknown degradation products were identified as (DP-I) 1-(2-(2-hydroxy-3-(isopropylamino)propoxy)-5-(amino)phenyl)ethanone, (DP-II) N-(4-(2-hydroxy-3-(isopropylamino)propoxy)-3-acetylphenyl)acrylamide, (DP-III) 1-(2-(2-hydroxy-3-(isopropylamino)propoxy)-5-(hydroxymethyl...
Source: Journal of Pharmaceutical Analysis - Category: Drugs & Pharmacology Source Type: research