10.46243/jst.2020.v5.i04.pp215-222 registered

This study presents a unique method for the selective extraction of degradants from API using HPLC and online connection of a SCIEX QTRAP 5500 mass spectrometer with a triple quadrupole mass analyzer and PDA detector. Chromatography was employed using mobile phase ACN: 0.1% TEA (40:60) %v/v to separate all degradants on the Agilent Eclipse XDB (150 mm x 4.6 mm, 3.5 μ) column. It was discovered that the maximum absorption occurs at 220 nm, allowing for simultaneous detection unaffected by the placebo matrix. It was decided to approve the recommended RP-HPLC technique in accordance with the general ICH guidelines. The parameters that were considered adequate were specificity, linearity, LoD, LoQ, accuracy, precision, and robustness of validation. The suggested approach demonstrates excellent linearity and robust correlation over the range of 12.5–75 μg/mL. The precision tests' percent RSD was less than 2%, whilst the accuracy trials yielded consistent recoveries (95–105%). It may be possible to determine the inherent stability of the drug molecules in the present formulation by doing forced degradation tests and evaluating the degradation products generated under different stress conditions. By using MS/MS analyses, the generated degradants were further described and effectively isolated. Validation studies showed that the recently developed method is stable and sensitive to all degradants. Validation studies show that within the required operating range, the newly created approach was also linear, accurate, precise, robust, and selective.