Stability-indicating RP-HPLC method development and validation for determination of nine impurities in apixaban tablet dosage forms. Robustness study by quality by design approach |
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Authors: | Velusamy B. Subramanian Naresh Kumar Katari Thirupathi Dongala Sreekantha B. Jonnalagadda |
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Affiliation: | 1. Department of Chemistry, School of Science, GITAM deemed to be University Hyderabad, Medak, Telangana, India;2. School of Chemistry and Physics, College of Agriculture, Engineering and Science, Westville Campus, University of KwaZulu–Natal, Durban, South Africa;3. Aurex Laboratories LLC, East Windsor, NJ, USA |
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Abstract: | A quality by design (QbD) based high-resolution HPLC method is described for determination of impurities in apixaban (APX) in the tablet dosage form. Employing a simple and stability-indicating HPLC method, nine known impurities were quantified with good peak resolution. Mobile phase A (MP-A) was prepared with buffer and acetonitrile 90:10 v/v, while mobile phase B (MP-B) contained water and acetonitrile 10:90 v/v. The gradient program was 0 min, MP-A 75%, B 25%; 20 min, MP-A 65%, B 35%; 30 min, MP-A 40%, B 60%; 40min, MP-A 40%, B 60%; 42 min, MP-A 75%, B 25%; and 50 min, MP-A 75%, B 25%. The chromatographic separation was achieved using a Zorbax RX C18 250 × 4.6 mm column, 5 μm (1.0 ml min−1, 280 nm, 50 μl) and a column temperature of 40°C. Several separation studies were carried out using design of experiments to optimize the method. Validation results confirm the applicability of the developed method for quality analysis and stability studies of the regular product on the manufacturing stream. |
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Keywords: | apixaban impurities method development quality by design RP-HPLC validation |
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