Development and Validation of High Performance Liquid Chromatography Method for the Determination of Process Related Impurities in Dapoxetine Hydrochloride

A sensitive and stable High Performance liquid chromatographic method has been developed for the identification of three process related impurities viz impurity-A, impurity-B and impurity-C in Dapoxetine hydrochloride. The method was optimized based on the peak shape and resolution of impurity-A, impurity-B and impurity-C. Phenomenex Luna C18 column (250mm×4.6 mm, 5um) was used for optimization of the method. The mobile phase for A pump consisted of 0.1% trifluro acetic acid in water and for that of B pump it consisted of 0.1% trifluro acetic acid in acetonitrile. The method was validated as per International Conference of Harmonization (ICH) guidelines in terms of quantitation limit (QL), detection limit (DL), linearity, precision, accuracy, specificity and robustness. The QL and DL values for impurity-A were found to be 0.02% and 0.005%, for that of impurity-B were found to be 0.028% and 0.009% and for that of impurity-C were found to be 0.048% and 0.016% respectively, with respect to sample concentration. The method was linear within the range of QL to 200% for all the three impurities. Thus, the newly developed method was found to be accurate, efficient and stable. The characterizations of these impurities were carried out for the confirmation of respective structures using nuclear magnetic resonance spectroscopy (NMR). A degradation study was also performed for Dapoxetine hydrochloride.