LC and LC-MS/MS Studies for the Separation and Identification of Impurities and Degradation Products of Betaxolol

Anis Chmangui; Mehdi Safta; Mohamed Ridha Driss; Soufiane Touil; Sondes Bouabdallah

doi:10.1093/chromsci/bmae025

LC and LC-MS/MS Studies for the Separation and Identification of Impurities and Degradation Products of Betaxolol

J Chromatogr Sci. 2024 May 8:bmae025. doi: 10.1093/chromsci/bmae025. Online ahead of print.

Authors

Anis Chmangui¹, Mehdi Safta², Mohamed Ridha Driss¹, Soufiane Touil¹, Sondes Bouabdallah^{1

3}

Affiliations

¹ Laboratory of Hetero-Organic Compounds and Nanostructured Materials (LR18ES11), Department of Chemistry, Faculty of Sciences of Bizerte, University of Carthage, Jarzouna, 7021, Tunisia.
² National Institute of Research and Physicochemical Analysis, Technopark of Sidi Thabet, Sidi Thabet, 2020, Tunisia.
³ National High School of Engineering of Tunis (ENSIT), University of Tunis, Tunis, 1008, Tunisia.

PMID: 38717216
DOI: 10.1093/chromsci/bmae025

Abstract

Betaxolol (Bx) is a selective β1 receptor blocker used in the treatment of hypertension and glaucoma. The aim of the present work was to demonstrate an approach involving use of liquid chromatography (LC) and liquid chromatography-electrospray ionization mass spectrometry (LC-ESI/MS) for the simultaneous separation, identification and characterization of impurities and of degradation products of betaxolol without their isolation from the reaction mixtures. At optimum condition, and according to ICH guidelines, the limit of detection (LOD) and limit of quantification (LOQ) for Bx are found to be 5.46 and 16.54 μg mL-1, respectively. However, the LOD and LOQ for the major degradation product P6 were 2.15 and 6.53 μg mL-1. Betaxolol was subjected to hydrolytic (acidic and basic) and oxidative, stress conditions according to International Conference on Harmonization (ICH) guideline Q1A (R2), and as results, the drug was found to be labile in acidic, basic and oxidative stress conditions. Based on LC-ESI/MS analysis, the found results revealed that Bx decomposes in acidic, basic and oxidizing environments. All degradation products were identified with the help of their fragmentation pattern and the masses obtained upon the MS analysis.