Development and Validation of Stability-Indicating HPTLC Method for Mirabegron with Identification, and Characterization of Degradant by ESI-MS

The objective of the present study is to elucidate the structure of the degradants of Mirabegron by High-performance thin layer-Tendom mass spectrometry, advising its structure elucidation, identification of its pathways of degradation, and establishing a stability-indicating assay method. In the present study, comprehensive stress testing of Mirabegron was carried out according to ICH guideline Q۲ (R۲) and a stability-indicating assay method for the identification, quantification, and characterization of the drug Mirabegron and its degradants, and the founding of pathways of acidic and alkaline degradation. Stability studies were conducted using stress conditions such as hydrolytic, oxidative, thermal, and photolytic conditions and degradation products were investigated and characterized by HPTLC-MS as per ICH guideline Q۲ (R۲)]. The current study develops a novel analytical method for separating drugs from the degradation products that is formed under stress conditions by utilizing Aluminum plates precoated silica gel G ۶۰F۲۴۵ and n-Butanol: Methanol: Water: Ammonia (۶:۲:۲:۰.۲ v/v/v/v) optimized mobile phase. Quantification was done by densitometric analysis at wavelength ۲۵۷ nm. The method produced a resolved band for Mirabegron (Rf) (۰.۶۷ ± ۰.۰۱۴). A linearity study was done in the range of ۱۰۰-۷۰۰ ng/band and the linear relationship in the calibration curve with R۲= ۰.۹۹۷. The Limit of Detection and Limit of Quantification was ۰.۰۴۷ and ۰.۱۴۳ ng/band obtained, respectively. Developed and validated a new, specific, sensitive, and economical High-Performance Thin-Layer Chromatography method for Mirabegron a β ۳-receptor agonist for the determination in bulk powder and tablet. Precision and recovery results as per as the International Conference on Harmonization guidelines were found to be in good range. The molecule is sufficiently stable under various stress tests. However, the degradation product formed in alkaline and oxidative hydrolytic stress has been used in LC-Q-TOF-MS/MS for characterization and the degradation pathway of the drug have been proposed.

کلیدواژه ها:

Mirabegron High ، performance thin layer chromatography Degradant Stability ، indicating assay method Characterization