Abstract

DEVELOPMENT AND VALIDATION OF A STABILITY INDICATING RP-HPLC METHOD FOR EDOXABAN TOSYLATE MONOHYDRATE USING QBD APPROACH

Yash Khedekar*, P. D. Hamrapurkar and Sushant Kaple

Abstract

QbD(Quality by Design) has gained importance in the analytical method development. It involves the optimization of the critical parmaters and to evaluate their effect on the critical quality attributes. An attempt was to develop and validate a in bulk form. The Box- Behnken design was used for the Qbd approach in which the screening was done on the critical parameters i.e(Buffer pH, %ACN and flowrate) and their effects on the variable responses i.e(Retention time, NTP and Asymetry factor) was evaluated. The developed method was validated according to International Conference on Harmonization guideline with respect to accuracy, precision, specificity, linearity, solution stability and system suitability. For this, an isocratic condition of mobile phase comprising buffer of 0.01 M sodium acetate with pH 4.0 and acetonitrile in a ratio of 70:30, v/v at a flow rate of 1.0 mL/minute over Qualisil BDS C18, 250 mm×4.6 mm×5 μm column at 28 C temperature was maintained. The detection was done using a PDA detector at 290nm. The method showed excellent linear response with correlation coefficient (R2) values of 0.999 for Edoxaban tosylate monohydrate, which was within the limit of correlation coefficient (R2 ≥ 0.995). The percent recovery was found within the acceptance limit of 98.0% to 102.0%. The %RSD for precision studies was found to be less than 2%. The Limit of Detection(LOD) and Limit of Quantification(LOQ) was found be 0.2μg/ml and 0.5 μg/ml respectively.

Keywords: Edoxaban Tosylate Monohydrate, Stability indicating method, Validation, QbD.