Application of Quality by Design in the Development of HPTLC Method for Estimation of Anagliptin in Bulk and inhouse Tablets

Abstract

This paper comprehends systematic Quality by Design (QbD) based development of
Normal-Phase High-Performance Thin-Layer Chromatography (NP-HPTLC) method for
qualitative and quantitative estimation of anagliptin in bulk and in-house tablets.
Chromatographic separation was executed out on aluminum backed Silica gel F254 plates
using dichloromethane: methanol (9.2:0.8 v/v) as a mobile phase. Densitometry scanning
was accomplished at 248 nm. Quality target method profile was defined and critical
analytical attributes (CAAs) for the HPTLC method set aside. The mobile phase ratio and
saturation time were determinate as critical method parameters (CMPs) and systematically
optimized using Central composite design, evaluating for CAAs, namely retention factor
(Rf), Peak-area and Peak-height. Statistical modelization was implemented followed by
response surface analysis for comprehending plausible interaction(s) among CMPs. Search
for optimum solution was conducted through numerical and graphical optimization for
demarcating the design space. The described method was linear. The precision, ruggedness,
and robustness values were also within the prescribed limit. The studies successfully
demonstrate the utility of QbD approach for developing the highly sensitive HPTLC method
with enhanced method performance.