Development and validation of a stability-indicating reversed phase high-performance liquid chromatography method for
1Department of Applied Pharmaceutical Sciences and Clinical Pharmacy, Faculty of Pharmacy, Isra University, P.O. Box 22, Amman 11622, Jordan; Department of Pharmaceutical Sciences, Eugene Applebaum College of Pharmacy and Health Sciences, Wayne State University, Detroit, MI 48202, USA; Department of Pharmaceutical Sciences, School of Pharmacy, Northeastern Illinois University, Chicago, IL 60625, USA.
Rivaroxaban is an anticoagulant medication that targets a key stage in the blood clotting process, preventing the formation and growth of clots. It is commonly used to prevent thrombosis or inhibit the enlargement of existing clots. Rivaroxaban functions as a Factor Xa inhibitor and is indicated for: reducing the risk of stroke and systemic embolism in patients with non-valvular atrial fibrillation, treating deep vein thrombosis (DVT) and pulmonary embolism (PE), as well as reducing the risk of recurrent DVT and PE, and prophylaxis of DVT, which may lead to PE in patients undergoing knee or hip replacement surgery. A robust, precise, and selective reversed-phase high-performance liquid chromatography (HPLC) method was developed and validated for analyzing Rivaroxaban in raw materials. Isocratic elution at a flow rate of 1 mL/min was performed using a Thermo ODS Hypersil C18 column (4.6 × 250 mm, 5 μm) at ambient temperature. The mobile phase consisted of monobasic potassium phosphate at pH 2.9 and acetonitrile in a 70:30 (v/v) ratio, with UV detection at 249 nm. Linearity was established in the concentration range of 50-1000 ppm (r2 = 0.999), and the retention time for Rivaroxaban was approximately 12 min. The percentage relative standard deviation (RSD) for precision and accuracy was consistently below 2.0 %. Rivaroxaban was subjected to forced degradation under various conditions, including acid and base hydrolysis, hydrogen peroxide oxidation, heat, and UV light exposure. The developed method was validated for specificity, robustness, linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ), following International Conference on Harmonisation (ICH) guidelines. The LOD for impurities and degradants was found to be 0.3 ppm, with an LOQ of 1 ppm.
Rivaroxaban is an anticoagulant medication that targets a key stage in the blood clotting process, preventing the formation and growth of clots. It is commonly used to prevent thrombosis or inhibit the enlargement of existing clots. Rivaroxaban functions as a Factor Xa inhibitor and is indicated for: reducing the risk of stroke and systemic embolism in patients with non-valvular atrial fibrillation, treating deep vein thrombosis (DVT) and pulmonary embolism (PE), as well as reducing the risk of recurrent DVT and PE, and prophylaxis of DVT, which may lead to PE in patients undergoing knee or hip replacement surgery. A robust, precise, and selective reversed-phase high-performance liquid chromatography (HPLC) method was developed and validated for analyzing Rivaroxaban in raw materials. Isocratic elution at a flow rate of 1 mL/min was performed using a Thermo ODS Hypersil C18 column (4.6 × 250 mm, 5 μm) at ambient temperature. The mobile phase consisted of monobasic potassium phosphate at pH 2.9 and acetonitrile in a 70:30 (v/v) ratio, with UV detection at 249 nm. Linearity was established in the concentration range of 50-1000 ppm (r2 = 0.999), and the retention time for Rivaroxaban was approximately 12 min. The percentage relative standard deviation (RSD) for precision and accuracy was consistently below 2.0 %. Rivaroxaban was subjected to forced degradation under various conditions, including acid and base hydrolysis, hydrogen peroxide oxidation, heat, and UV light exposure. The developed method was validated for specificity, robustness, linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ), following International Conference on Harmonisation (ICH) guidelines. The LOD for impurities and degradants was found to be 0.3 ppm, with an LOQ of 1 ppm.
