Selective Separation and Mass Spectral Characterization of Degradants in Viloxazine by LC-MS/MS

Abstract

This research describes a novel technique for the selective separation of degradants from API employing HPLC and online coupling of a triple quadrupole mass analyzer and PDA detector with a SCIEX QTRAP 5500 mass spectrometer. Chromatography was used to separate all degradants on the column Agilent eclipse XDB (150 mm x 4.6 mm, 3.5 μ) with mobile phase ACN: 0.1% TEA (40:60) %v/v. The highest absorption was found to occur at 220 nm, which allows for simultaneous detection without being impacted by the placebo matrix. According to the general ICH recommendations, the suggested RP-HPLC method was accepted. All of the metrics- specificity, linearity, LoD, LoQ, accuracy, precision and robustness of validation were deemed sufficient. The proposed method exhibits strong correlation and great linearity over the range of (12.5–75 μg/mL). The accuracy trials produced consistent recoveries (95–105%), while the precision experiments' percent RSD was less than 2%. The intrinsic stability of the drug molecules in the current formulation could be ascertained by conducting forced degradation studies to assess the degradation products produced under various stress settings. The degradants produced were well separated and further characterized by MS/MS studies. The newly devised approach was demonstrated to be stable and sensitive to all degradants during validation tests. Validation trials demonstrate that the newly developed method was also accurate, precise, resilient, selective, and linear within the necessary operating range.