Quality by Design based pareto charts responses Evaluation approach for a Validated Stability-indicating RP-HPLC assay Method for sunitinib and its process related impurities in Oral Dosage Forms

Abstract

For sunitinib (SUN) and its associated impurities, a simple and rapid stability-indicating liquid chromatographic assay technique was developed. The SUN related impurities in the completed oral dose forms were detected and assessed utilizing the high-pressure liquid chromatography with help of analytical quality by design (AQbD) approach. Impurity quantification necessitates a more comprehensive approach to analytical technique generation. The pareto charts evaluation technique, that is dependent on quality by design, enables for the evaluation of many analytical aspects and their consequences with a small series of investigations. A spiked sample mixture was separated to six specified known SUN impurities as well as undefined degradation products with significant chromatographic resolution. The separation was undertaken on a column of C18 (150 mm x 4.6 mm, 3.5 µm) with a mobile phase flow volume of 1.0 ml in a minute in a gradient elution manner. The mobile phase component A was composed of 20 mM KH2PO4 (pH 7.0), while the mobile phase component B was acetonitrile. Compound detection was conducted out at 268 nm, with the column temperature kept fixed at 40 oC. Stress degradation samples were subjected to oxidation, acid, base, thermal, and photolysis consistent with the endorsements of “International Conference on Harmonization” (Q2) methodology. The established method for SUN and its associated impurities assessment was validated as stability indicating, precise, robust, specific, rugged, and accurate.