ANALYTICAL QUALITY BY DESIGN APPROACH IN RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF DUVELISIB
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.
This work is licensed under a Creative Commons Attribution 4.0 International License.
The publication is licensed under CC By and is open access. Copyright is with author and allowed to retain publishing rights without restrictions.