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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
Author(s) -
Subramanian Velusamy B.,
Katari Naresh Kumar,
Dongala Thirupathi,
Jonnalagadda Sreekantha B.
Publication year - 2020
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.4719
Subject(s) - chemistry , chromatography , high performance liquid chromatography , acetonitrile , resolution (logic) , impurity , quality by design , analytical chemistry (journal) , particle size , organic chemistry , artificial intelligence , computer science
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 C 18 250 × 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.