Method Development and Validation of a Reversed- Phase HPLC Method for Assay and Related Substances of Prednisolone Sodium Phosphate

摘要

Prednisolone Sodium Phosphate active pharmaceutical ingredient (API) is a white or slightly yellow powder with a molecular formula of C21H27Na2O8P and a molecular weight of 484.39. It is a corticosteroid with a wide variety of uses such as: the control of allergies, skin disorders, edema, hormone disorders, digestive diseases, blood disorders, neoplasm, nervous system dysfunction, eye diseases, respiratory diseases, and rheumatoid arthritis. The decision to develop an HPLC for the determination of assay and related substances in prednisolone sodium phosphate API is because, at the time, there was no USP monograph method. Additionally, most methods published were outdated and not practical for use. These observations were the motivating factors that led to the decision to develop and validate a method that is simple, robust, specific, accurate, precise, and reproducible. Finally, the goal was for it to be a reversed-phase HPLC method, with reasonable run time to determine the assay and related substances of prednisolone sodium phosphate API.Method development is a process of developing a method where compounds of interest can be separated and quantified in the presence of other sample components. The main objective of the study was to develop a simple and reliable reversed-phase HPLC method for the determination of assay and related substances of prednisolone sodium phosphate API. The expectation is that the method will be capable of quantifying related substances of prednisolone sodium phosphate impurities and degradants under long-term stability studies.Analytical method validation is the procedure where various parameters are studied to verify if a method is suitable and reliable for its intended use. Several validation studies were performed to evaluate the HPLC method developed in this study. They follow the guidelines set by the International Conference on Harmonization (ICH) along with the requirements set the Food and Drug Administration (FDA). The validation parameters studied are system suitability, solution stability, robustness, specificity, linearity, limit of quantitation (LOQ), limit of detection (LOD), accuracy, precision, and range.In this experiment, the method was validated according to ICH guidelines for the active pharmaceutical ingredient. All the validation parameters for the API met the acceptance criteria suggested by ICH guidelines listed in the previous paragraph. The method is easy to use, economic, precise, and ready for use.