DEVELOPMENT AND VALIDATION OF A STABILITY-INDICATING REVERSED PHASE ULTRA PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR THE QUANTITATIVE ANALYSIS OF RALOXIFENE HYDROCHLORIDE IN PHARMACEUTICAL DOSAGE FORM

A rapid, specific, and sensitive ultra-performance liquid chromatographic (UPLC) method for quantitative analysis of raloxifene in bulk drug and pharmaceutical formulations has been developed and validated as per the guidelines laid by ICH. The chromatographic separation of raloxifene was achieved on a Waters Acquity BEH C-18, 50 x 2.1 mm, 1.7 mu m column with mobile phase containing a gradient mixture of solvent A (0.1% of Formic acid in water) and solvent B (acetonitrile). The method was linear in the range of 0.1-50 mu g/mL (r(2) = 0.9998) and having a run time of 6 min, which allows for a large number of samples to be analyzed in less time. The analyte was monitored at 287 nm. The method was validated according to the ICH guidelines with respect to linearity, precision, accuracy, limit of detection (LOD), lower limit of quantification (LLOQ), specificity, and robustness. Forced degradation studies were also performed for raloxifene bulk drug samples to demonstrate the stability-indicating aspect of the UPLC method. Degradation was found to occur in reductive condition only while the drug was stable to oxidation, alkaline, acidic, photolytic, and hydrolytic stress conditions. The developed method was applied for the assay of raloxifene formulations like tablets and nanoparticulate formulation.