ANALYTICAL QUALITY BY DESIGN APPROACH IN RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF DUVELISIB

Abstract

Objective: A simple, accurate and robust RP-HPLC method was developed and validated for the estimation of Duvelisib by using Analytical Quality by Design (AQbD) approach.

Method: The critical method parameters (CMP) were systematically optimized using Box-Behnken design (BBD). The CMP’s selected were % Organic phase composition, column temperature and flow rate. The critical quality attributes investigated were retention time and theoreticalplates.

Results:Chromatographic separation was accomplished on Agilent C 18(150×4.6 mm, 5 µm) column at 32.6⁰C. The optimized and predicted data from Design Expert software consisting of mobile phase 0.1 % OPA(46.3%): Acetonitrile (53.7%), pumped at a flow rate of 0.91ml /min at 32.6⁰C gave the highest desirability function of 1.The retention time of the drug was found to be 2.85min. The developed method was validated as per ICH Q2 (R1) guidelines.

Conclusion:Based on the ANOVA values the selected models were found to be significant with p< 0.05. The results of the validation parameters were within the acceptable limit.The stability of the drug was examined under different stress conditions forcibly and significant degradation was found in acidic condition.