Development and Validation of Stability Indicating RP-HPLC Method on Core Shell Column for Determination of Degradation and Process Related Impurities of Apixaban—An Anticoagulant Drug

• Published in: American journal of analytical chemistry Vol. 6; no. 6; pp. 539 - 550
• Main Authors: Landge, Shashikant B., Jadhav, Sanjay A., Dahale, Sunil B., Solanki, Pavankumar V., Bembalkar, Saroj R., Mathad, Vijayavitthal T.
• Format: Journal Article
• Language: English
• Published: 01.05.2015
• Subjects: Analytical chemistry; Anticoagulants; Arrays; Columns (process); Degradation; Drugs; Impurities; Run time (computers)
• ISSN: 2156-8251; 2156-8278
• DOI: 10.4236/ajac.2015.66052

A rapid, specific, sensitive, and precise reverse-phase HPLC method for the quantitative determination of process related and degradation impurities of Apixaban, an anticoagulant drug is described. The developed RP-HPLC method was successfully applied to the analysis of both Apixaban drug substance and drug product. The chromatographic separation was achieved on a Sigma-Aldrich's Ascentis Express C18 (4.6 mm x 100 mm, 2.7 mu ) HPLC column with a runtime of 40 min. Mobile phase-A and mobile phase-B were phosphate buffer and acetonitrile respectively. The column oven temperature was set at 35 degrees Celsius and photodiode array detector was set at 225 nm. Nine process related impurities (Imp-1 to Imp-9) have been detected in test sample of Apixaban, by using newly developed RP-HPLC method. Forced degradation study was carried out under acidic, alkaline, oxidative, photolytic and thermal conditions to demonstrate the stability-indicating nature of the developed RP-HPLC method. The developed method was validated as per ICH guideline, and found to be specific, precise, sensitive and robust.