DEVELOPMENT AND VALIDATION OF STABILITY INDICATING HPTLC METHOD FOR ESTIMATION OF APIXABAN IN PHARMACEUTICAL FORMULATIONSAbstract
A simple, accurate, precise, and rapid high-performance thin-layer chromatographic (HPTLC) method for determination of Apixaban (API) in bulk drug and the pharmaceutical formulation was developed and validated. The separation was performed on aluminum plates, pre-coated with silica gel 60F254 as the stationary phase using toluene: methanol (7:3 v/v), as mobile phase. Densitometric measurement of the API was carried out at 290 nm. The retention factor (Rf) was found to be 0.62 ± 0.04. The method was successfully validated as per International Conference on Harmonization (ICH) guidelines Q2 (R1). The calibration curve was linear in range 50-300 ng/band. The limits of detection and quantitation were 0.272 and 0.824 ng/band, respectively. Accuracy and precision of the proposed method were evaluated by recovery studies and intra-day and inter-day precision studies, respectively (standard deviation for precision studies was found to be less than 2). The developed method was used to analyze marketed formulation samples (tablet) of the API. The API was subjected to various stress conditions as per ICH Q1A (R2) guidelines. In stress studies, the drug showed significant degradation during acid, alkaline hydrolytic, and oxi-dative conditions. As the method could effectively separate the drug from their degradation products, it can be used as a stability indicating method.
S. V. Warghade * and K. G. Bothara
Department of Pharmaceutical Chemistry, STES’s Smt. Kashibai Navale College of Pharmacy, Kondhwa, Savitribai Phule Pune University, Pune, Maharashtra, India.
06 November 2018
09 March 2019
16 March 2019
01 July 2019