Characterization and Analytical Method Validation for Potential Impurities of a Merchantability Drug Substance Fluoxetine HCl

Abstract

A new selective and sensitive high-performance liquid chromatography (HPLC) method was developed for the quantification of potential impurities in fluoxetine hydrochloride. Chromatographic separation was achieved on an end-capped octadecylsilyl silica gel (Gemini-C18 150 mm × 4.6 mm, 3.0 μm) using a gradient program with triethylamine, methanol, and water as the mobile phase at a flow rate of 1.0 mL/min and monitored at 215 nm. The run time was 60 min. The method was validated to fulfill International Conference on Harmonization (ICH Q2(R2)) requirements, and this validation included specificity, precision, linearity, limit of detection (LOD), limit of quantification (LOQ), and accuracy. The calibration curve was linear over the concentration range from LOQ to 120% with respect to sample concentration. The accuracy of the method is within the acceptable limit of 80%–120%. The results obtained for all parameters were within the acceptance criteria. So, this method can be employed for the regular analysis of potential impurities in the fluoxetine hydrochloride API.