Spectroscopic Substantiation for the Identification of Degradants by Q-TOF Micromass (ESI-MS) in Bisoprolol Fumarate with an Inventive Validation Approach for Stability Indicating HPLC Method.

Background: Stability studies, stress testing of drug substances and finished drug product is obligatory due to the guidelines by the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) and other Regulatory Authorities. Materials and Methods: In the present work the selective Beta-1 receptor blocker, Bisoprolol fumarate was subjected to the forced degradation studies which includes hydrolysis (acidic, basic and neutral), oxidative, photolytic and thermal degradation. The drug was stable under light and basic and neutral medium. Results: The major findings in the presented work are the degradation products formed in the course of thermal degradation. The complete thermal degradation products were identified by High Performance Liquid Chromatography, Quadrupole-Time of Flight micromass (Electronspray Ionization-Mass Spectroscopy). The chromatographic conditions opted for the study includes Cosmosil C-18 column (4.6ID*250mm) with mobile phase consisting of methanol: phosphate buffer (pH 3.5 adjusted with orthophosphoric acid): Acetonitrile (45:35:20). Conclusion: The stability indicating method was validated as per the International Conference on Harmonization guidelines. The use of superior statistical tools for validation ensures the efficiency, quality and reproducibility of the presented method. Results obtained were agreeable and ensured the quality and reproducibility of the method. [ABSTRACT FROM AUTHOR]