Application of quality by design in the development of HPTLC method for estimation of anagliptin in bulk and in-house 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.