Abstract

ANALYTICAL DEVELOPMENT AND VALIDATION OF HPTLC METHOD FOR DETERMINATION OF SELEXIPAG IN BULK AND FORMULATIONS

S. Satheshkumar* and V. Muruganantham

ABSTRACT

The present research work deals with analytical method development and validation of a novel, accurate and precise method for the selexipag in bulk and formulation by using high-performance thin layer chromatography (HPTLC). The method employed TLC aluminium plates precoated with silica gel 60F254 as the stationary phase. The solvent system consisted of Tolene: Ethyl Acetate: Ethanol (4:4:2, v/v/v). The system was found to give a compact spot for selexipag with Rf value of 0.44 ±0.05. Densitometric analysis of selexipag was carried out in the absorbance mode at 300nm. The linear regression analysis data for the calibration plot showed a good linear relationship with r2 = 0.9998 with respect to peak area in the concentration range of 100-800 ng/spot. Complete validation was carried out for precision (inter-day, intra-day and repeatability), accuracy, limit of detection (LOD), limit of quantification (LOQ), specificity, robustness and stability as per International Conference on Harmonization (ICH) guideline. The limits of detection and quantitation were 26.88 and 81.44 ng/spot, respectively. All the data were analyzed statistically. This proposed method could also be useful for studying the selexipag degradation pattern and routine analysis in quality control laboratories for marketed tablet formulation at low cost.

Keywords: HPTLC, Selecipag, Validation, ICH guideline, Formulation.