Sensitive and validated UPLC-MS/MS method for the identification and characterization of forced degradation products for felodipine

Abstract

A rapid, stability indicating reverse phase liquid chromatographic method was developed for the determination of purity of Felodipine in active pharmaceutical substance form in the presence of its impurity and its degradation products. To develop the method which is also compatible to liquid chromatographic mass spectroscopic technique. The developed method is also used to determine the assay of Felodipine in bulk drug form. The drug is subjected to various stress conditions like acidic, basic, oxidation, UV light and thermal conditions. Considerable degradation was observed during base hydrolysis. Two degradation products were identified. The Waters Acquity UPLC BEH C18, 2.1 × 100 mm, 1.7 µm Column was used to achieve chromatographic separation. The gradient conditions, diluent and injection volume were optimized to achieve the acceptable resolution between impurities and its degradation products from Felodipine and to get good peak shapes. The masses were determined for main compound and its identified degradation products. Further, the characterization studies for main compound and its degradation products were performed using LCMSMS Q-TOF.

Analytical method validation for tenofovir alafenamide and known impurities

“…Specificity is achieved by evaluating the absence of interfering peaks at the retention time of TAF and its specified impurities when compared to blank diluents. The method also must demonstrate clear resolution between the peaks for TAF and its known impurities, further substantiating its specificity (Ajay et al, 2023).…”

“…Recent advancements in pharmaceutical research have witnessed a concerted effort to enhance analytical methodologies and validation techniques. Several noteworthy studies have surfaced in this pursuit, including sensitive UPLC-MS/MS methods for the identification of forced degradation products in felodipine (Ajay Babu et al, 2023), analytical method development and validation for Favipiravir in bulk and pharmaceutical forms (Ali et al, 2021), and the exploration of advanced techniques for Tenofovir analysis in anti-HIV pharmaceuticals (Avhad et al, 2023). Additionally, researchers have focused on the simultaneous quantification of related substances in combination with antiretroviral drug products (Balakrishnan et al, 2013), understanding degradation mechanisms for capmatinib (Bhangare et al, 2023), and comprehensive studies on Tenofovir Disoproxil Fumarate (Bora et al, 2012).…”