Multivariate UV-Chemometric and HPLC-QbD Method for Simultaneous Estimation of Vardenafil and Dapoxetine in Active Pharmaceutical Ingredients and its Marketed Formulation

Background: This manuscript focuses on Novel multivariate UV-chemometric method and HPLC-QbD method for simultaneous determination of Vardenafil (VR) and Dapoxetine (DP) in active pharmaceutical ingredient and their marketed formulation. To the best of our knowledge, there is no literature data on multivariate methods for the same. Methods: The spectrophotometric data were processed by CLS, PCR, PLS and MLR methods in order to determine the active substances, without prior separation from tablet marketed formulation. Analytical figures of merit, such as sensitivity, selectivity, analytical sensitivity, LOD, and LOQ were determined. In HPLC-QbD, four critical factors were selected after screening and boxbehnken design was applied for optimization. Twenty-five experiments were done, and a quadratic model was used for all response variables. Desirability plot, surface plot, design space, and three-dimensional plots were calculated. Results: For Chemometrics, wavelength range selected was 202 nm - 326 nm at 2 nm intervals, hence 59 wavelength points were selected in such a way that minimum RMSEC and RMSECV values were obtained at multiple wavelengths. HPLC-QbD optimized conditions were; Phenomenex C8 column (250 x 4.6 mm, 5 μm), acetonitrile: buffer (ammonium acetate buffer at pH 2.7 with acetic acid) (40:60, v/v) as a mobile phase at flow rate of 0.9 mL/min, 239 nm wavelength and 20°C temperature. Conclusion: The developed methods were validated and successfully applied for simultaneous determination of VR and DP in tablet dosage form. The results obtained by UV-Chemometric methods were statistically compared with an HPLC-QbD method, which concludes both the methods can apply for tablet analysis.