ANALYTICAL QUALITY BY DESIGN (AQbD)-BASED RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF AZILSARTAN

Abstract

A good and effective consistent analytical method of quantitative determination of azilsartan in
bulk and tablet dose forms was developed by the application of Analytical Quality by Design
(AQbD) principles. A Central Composite Design (CCD) has been applied to optimize the method
and to determine the impact of the critical method parameters on the chromatographic
performance. Separations were done in Agilent Zorbax C18 column (250 mm × 4.6 mm, 5 μm)
using a mobile phase of phosphate buffer and methanol in the proportions of 50:50 (v/v) at a flow
rate of 1.0 mL/min. The wavelength of detection was 256 nm, and the retention time of azilsartan
was about 2.9 minutes. The constructed method was confirmed as per the ICH Q2(R2) guidelines
as it exhibits excellent linearity (r2 = 0.9999), accuracy, precision, specificity and robustness. The
percentage relative standard deviation (percentage RSD) was less than 2.0 percent indicating that it
is highly precise and recovery studies yielded an average recovery of 100.36 percent. The limit of
detection (LOD) and the limit of quantitation (LOQ) were calculated to be 3.26 μg/mL and 9.86
μg/mL, respectively, calculated per ICH Q2(R2) using standard deviation and slope method
(sigma/S). The proposed approach is easy, quick, and cost-effective, which is why it can be applied
to routine studies of azilsartan in pharmaceutical preparations. The use of AQbD offered a better
understanding of the method and its robustness that could be successfully implemented in the area
of quality control.