ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF TADALAFIL AND MACITENTAN BY USING RP-UPLC IN BULK AND PHARMACEUTICAL DOSAGE FORM AND FD CHARACTERIZATION BY USING LCMS

ABSTRACTThe current investigation was pointed at developing and progressively validating novel, simple,responsive and stable RP-UPLC method for the simultaneous measurement of active pharmaceutical ingredients of Macitentan and Tadalafil. A simple, selective, validated and well-defined stability that shows isocratic RP-UPLC methodology for the simultaneous determination of Macitentan and Tadalafil and FD characterization by using LCMS. The chromatographicstrategy utilized X-Bridge C18 column of dimensions (50x4.6mm, 2.1μm), using isocraticelution with a mobile phase of acetonitrile and 0.1% TEA pH-2.5/formic acid (40:60). A flowrate of 0.5 ml/min, injection volume of 5μl and a detector wavelength of 266 nm utilizing thePDA detector were given in the instrumental settings. LOD and LOQ for the active ingredientwere established with respect to test concentration. The calibration chart plotted was linear witha regression coefficient of R2 > 0.999, means the linearity was within the limit. Specificity,linearity, accuracy, robustness, ruggedness were determined as a part of method validation andthe results were found to be within the acceptable range. Validation of the proposed method wascarried out according to an international conference on harmonization (ICH) guidelines. Theproposed method to be fast, simple, feasible and affordable in assay condition. During stabilitytests, it can be used for routine analysis of production samples and to verify the quality of drugsamples during stability studies.