Analytical Development and Validation of a Stability-Indicating Method for the Estimation of Impurities in Budesonide Respules Formulation

Abstract

A short selective, precise, accurate and sensitive stability-indicating LC-MS/MSn method was developed for the quantitative determination of process-related impurities and degradation products of Budesonide in pharmaceutical respules formulations. During the stress study, the degradation products of Budesonide were well-resolved from Budesonide and its impurities and the mass balances were found to be satisfactory in all the stress conditions, thus proving the stability-indicating capability of the method. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, ruggedness and robustness. During the stability analysis of the drug product, all known impurities were detected by the above stability-indicating method. The flow rate was 0.8 ml/min and effluent was monitored at 247nm. Retention time was found to be 17.329±0.75 min and18.439±0.65 min of epimers (22R and 22S)respectively. The LOD and LOQ values for were found to be 0.20936 (μg/ml) and 0.6344 (μg/ml) respectively.