Stability-indicating RP-HPLC method development and validation for quantitative determination of Dexlansoprazole in bulk drug and dual delayed-release capsule

Overview

This study reports the development and validation of a stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method for quantitative determination of dexlansoprazole in bulk drug and dual delayed-release capsule formulations. Dexlansoprazole, a proton pump inhibitor, requires analytical methods capable of detecting degradation products while accurately quantifying the active pharmaceutical ingredient in pharmaceutical preparations. The method utilized an Inertsil ODS C18 column with a mobile phase consisting of phosphate buffer at pH 7.0 and acetonitrile in a 55:45 volumetric ratio, with UV detection at 285 nm and a flow rate of 1.0 ml/min. Validation followed International Council for Harmonisation (ICH) guidelines, encompassing specificity, linearity, precision, accuracy, robustness, range, and system suitability parameters. The validated method addresses the need for routine quality control analysis of dexlansoprazole in pharmaceutical manufacturing and regulatory testing environments.

Methods and approach

Chromatographic separation was performed on an Inertsil ODS C18 column measuring 250.0 x 4.6 mm with 5.0 micrometer particle size. The mobile phase composition of phosphate buffer pH 7.0 and acetonitrile at 55:45 volumetric ratio was delivered at a flow rate of 1.0 ml/min, with detection performed by UV spectrophotometry at 285 nm. The method validation protocol adhered to ICH guidelines and evaluated multiple parameters including specificity to assess interference from excipients and degradation products, linearity across a specified concentration range with correlation coefficient determination, precision through relative standard deviation measurements, accuracy studies, and robustness testing under deliberate variations in analytical conditions. System suitability parameters were also assessed to ensure the chromatographic system's performance capability for the intended application in both bulk drug and capsule dosage form analysis.

Key Findings

The validated method demonstrated excellent specificity with no detectable interference from pharmaceutical excipients or degradation products formed under stress conditions. Linearity was confirmed over the selected concentration range, yielding a high correlation coefficient indicative of proportional detector response. Precision and accuracy evaluations produced relative standard deviation values within acceptable limits as defined by ICH guidelines, confirming the method's reliability for quantitative determination. Robustness testing revealed consistent analytical performance despite small deliberate variations in method parameters, demonstrating the method's resilience to minor procedural deviations that may occur during routine implementation. These results collectively establish the method's suitability as a stability-indicating assay capable of distinguishing dexlansoprazole from its degradation products while providing accurate quantitative data.

Implications

The validated RP-HPLC method provides a reliable analytical tool for routine quality control analysis of dexlansoprazole in both bulk pharmaceutical material and capsule formulations. Its stability-indicating nature enables simultaneous assessment of drug stability and purity, which is essential for pharmaceutical manufacturing, storage stability studies, and regulatory compliance. The method's demonstrated specificity, accuracy, precision, and robustness make it suitable for implementation in quality control laboratories without requiring extensive method development or optimization. The validation against ICH guidelines ensures international acceptance and regulatory compliance, facilitating its adoption in pharmaceutical testing environments where standardized, validated analytical procedures are required for batch release and stability monitoring programs.