VALIDATION OF ANALYTICAL METHODS IN A PHARMACEUTICAL QUALITY SYSTEM: AN OVERVIEW FOCUSED ON HPLC METHODS

Analytical validation has fundamental importance in the scope of Good Manufacturing Practice (GMP) for pharmaceutical products since it establishes scientific evidence that an analytical procedure provides reliable results. However, even with validation guidelines available it is very common to observe misunderstandings in the execution of validation and data interpretation. The misguided approaches of validation guidelines, allied with a disregard for the peculiarities of the analytical techniques, the nature of the sample, and the analytical purpose, have significantly contributed to oversights in analytical validation. This work aims to present a critical overview of the validation process in pharmaceutical analysis, addressing relevant aspects of various analytical performance parameters, their different means of accomplishment and limitations in face of the analytical techniques, the nature of the sample, and the analytical purpose. To help in the planning and execution of the validation process, some case studies are discussed, mainly in the area of high-performance liquid chromatography (HPLC).

分析验证在药品良好生产规范（Good Manufacturing Practice, GMP）范畴内具有根本性重要意义，因其可为分析方法获得可靠结果提供科学依据。尽管已有验证指南可供参考，但在验证执行与数据解读环节仍频繁出现认知误解。对验证指南的不当使用，加之忽视分析技术的特殊性、样本属性与分析目的，极大地加剧了分析验证中的疏漏问题。本研究旨在对药物分析中的验证流程开展批判性综述，系统阐述各类分析性能参数的相关要点、不同实现路径，以及其针对分析技术、样本属性与分析目的所存在的局限性。为助力验证流程的规划与执行，本文还探讨了若干案例研究，其中主要涉及高效液相色谱法（high-performance liquid chromatography, HPLC）领域。