Analytical Quality by Design Approach for the Development and Validation of Liquid Chromatographic Procedure for the Estimation of Abrocitinib

Abstract

Analytical quality by design-based HPLC procedure has been developed for the estimation of Abrocitinib in bulk and tablets. Design-Expert^®-13 was employed for Response Surface Methodology. ANOVA was applied for responses statistical analysis. Buffer pH, flow rate, % organic composition of mobile phase, column and organic modifier were considered as CMPs. Retention time, number of theoretical plates and tailing factor were considered as CQAs. The CMPs that have a significant impact on CQAs were screened utilizing a 12-run 2⁵ Plackett-Burman design. Following screening investigation, CMPs that have a substantial effect on the CQAs were selected and CMPs of HPLC procedure were optimized employing a 22-run 5³ central-composite design. The optimized procedure suggested by the desirability functions approach utilizing a 55.8:44.2 ratio pH 3.25 ammonium formate buffer and acetonitrile with 1.0 mL/min flow rate as a mobile phase, an Inertsil ODS (150×4.6 mm, 3.5 μm) column as a stationary phase with 5 mins run time resulting in maximum desirability, 1.000. At 3.575 min, Abrocitinib retention time was observed. The optimized procedure was validated and stress studies were executed in accordance to the ICHQ2(R1) and ICHQ1A guidelines respectively. In accordance with the literature, it is evident that this is the initial reported RP HPLC procedure for Abrocitinib estimation.