Quality by Design (QbD) based development and validation of RP-HPLC Method for Quantification of Silodosin and Mirabegron in Pharmaceutical Dosage Forms
A novel, stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the simultaneous quantification of Silodosin and Mirabegron in pharmaceutical formulations, employing a Quality by Design (QbD) approach. Chromatographic optimization yielded sharp, symmetrical peaks with satisfactory resolution under the selected mobile phase, column, and pH conditions. Validation followed ICH Q2(R1) guidelines, confirming excellent linearity (R² = 0.999) across the tested concentration ranges, high accuracy with recovery values of 98–99%, and precision with %RSD well below the acceptable limit. The method exhibited low limits of detection and quantification (LOD: 0.4 µg/mL for Silodosin and 1.3 µg/mL for Mirabegron; LOQ: 1.3 µg/mL and 4.3 µg/mL, respectively), reflecting high sensitivity. Robustness testing demonstrated stability under small, deliberate variations in chromatographic conditions, while specificity studies confirmed the absence of interference from excipients or degradation products. Forced degradation experiments revealed distinct separation of degradation peaks under acidic, basic, oxidative, photolytic, and thermal conditions, establishing the method’s stability-indicating nature. The validated procedure can be useful in terms of reliability, reproducibility and flexibility when utilized in routine quality control, release, testing, and stability evaluation of Silodosin and Mirabegron formulations.
