Optimization of HPLC-FLD Conditions Using Analytical Quality by Design Approach for Quantification of Silodosin in Pharmaceutical Dosage Form

Abstract

An HPLC-FLD method was developed using a surface response methodology for the quantification of silodosin in pharmaceuticals. The HPLC-FLD method was validated for accuracy, precision, working range, reproducibility, the limit of detection, the limit of quantification, and robustness. Analytical Quality by Design (AQbD) strategy was applied to develop an HPLC-FLD method for the quantification of silodosin in pharmaceuticals by using a central composite design methodology. Excitation and emission wavelengths with the highest fluorescence response for silodosin were determined by spectrofluorometric measurements at 256 nm and 456 nm, respectively. The parameters that have an impact on chromatographic separation and detection of silodosin were selected as pH, column temperature, and organic content of the mobile phase (acetonitrile %). A quadratic three-factor central composite design model consisting of 20 observations was used. The method showed good recovery and accuracy. The method was linear in the range of 0.1–40 µg/mL, with a high correlation coefficient (0.9991) and acceptable precision (RSD