ANALYTICAL QUALITY BY DESIGN APPROACH IN RP-HPLC METHOD DEVELOPMENT FOR THE ASSAY OF PITAVASTATIN IN TABLET DOSAGE FORM

Chromatographic method was developed according to Quality by Design (QbD) approach as per ICH Q8 (R2) guidelines for estimation of pitavastatin in pharmaceutical dosage form. By considering the current regulatory requirement for an analytical method development, a reversed phase high performance liquid chromatographic method for routine analysis of Pitavastatin has been optimized using analytical quality by design approach. Unlike routine approach, the present study was initiated with understanding of quality target product profile, analytical target profile and risk assessment for method variables that affect the method response. A liquid chromatography system equipped with a C₁₈ column (250 × 4.6 mm, 5 µ), a binary pump and photodiode array detector were used in this work. The experiments were conducted based on plan by central composite design, which could save time, reagents and other resources. Sigma Tech software was used to plan and analyses the experimental observations and obtain quadratic process model. The process model was used for predictive solution for retention time. The predicted data from contour diagram for retention time were verified actually and it satisfied with actual experimental data. The optimized method was achieved at 1.2 ml/min flow rate of using mobile phase composition of methanol and OPA in water at 80:20% v/v, pH adjusted to 6.5 adjusted with 10% ammonia. The method was validated and verified at flexible input variable level for high degree of robustness and system suitability during method transfer.