Spectroscopic characterization of selexipag and vismodegib active pharmaceutical ingredients and impurities, and analytical method development and validation by chromatographic methods

Selexipag drug active ingredient is used in the treatment of pulmonary arterial hypertension (PAH), a rare disease. Vismodegib is used in the treatment of basal cell carcinoma, a type of skin cancer. For this purpose, based on the ICH guideline for the generically produced Selexipag and Vismodegib pharmaceutical active ingredients, the relevant substances and the quantification method were developed and validated. Reverse-phase chromatography was studied due to the apolar nature of drug active ingredients. After determining the limits of active substances and impurities according to the ICH guide, the substances are spectroscopically; It was identified by 1H-NMR, 13C-NMR, FTIR, mass spectrometers. Standardization of the defined substances has been made and related compounds and quantifications have been made for the active pharmaceutical ingredients taken from the production batches. The methods have been successfully validated according to the ICH Q2(R1) guidelines. Thus; precise, accurate, stable and selective methods that can be used for routine analyzes in quality control laboratories have been obtained. Active pharmaceutical ingredients were subjected to harsh degradation conditions for stability and shelf life studies and analyzed simultaneously with validated related compounds and quantification methods. As a result of the study, two drugs showed that the active substance was stable under these conditions. No significant difference was observed between the accelerated six-month stability results either.