Quality by Design based Analytical method Development and Validation for the Estimation of Luliconazole in API and Pharmaceutical Dosage form.

ABSTRACT

A novel Quality by Design methodology was used to develop and validate a rapid, accurate, precise, simple, efficient and reproducible isocratic Reversed Phase-High Performance Liquid Chromatographic (RP-HPLC) method for the estimation of Luliconazole in bulk and pharmaceutical dosage form. Luliconazole was separated using Kromasil C18 column (250mm×4.6 mm, 5µm particle size), Shimadzu LC2030 HPLC system having UV detector and the mobile phase contained a mixture of 0.01M Ammonium acetate buffer and Acetonitrile (35:65). The flow rate was set to 1.2 ml/min with the responses measured at 294nm. The retention time of Luliconazole was found to be 3.092 min. Central composite design employed for design of experiment and optimization. Desirability value was found to be 0.723 and overall model was found to significant. Linearity was established for Luliconazole in the range of 20-120 µg/ml with correlation coefficient (r2=0.9995). Limit of detection (LOD) and limit of quantitation (LOQ) were evaluated and found to be 1.1700 and 3.5455 respectively. The accuracy values were found to be in the range of 98 –102% and every parameter found with in limit. Validation parameters were evaluated for the method according to the International Conference on Harmonization (ICH) Q2 R1 guidelines. This method can be used for the estimation and analysis of Luliconazole drug in active pharmaceutical ingredients and pharmaceuticals.

Keywords: 3 level factorial designs, Luliconazole, Development, Validation.