CDER色谱方法验证.docx

色谱方法验证目录Ⅰ简介Ⅱ色谱法分类高效液相色谱法（HPLC）手性色谱法离子交换色谱法离子对色谱法正相色谱法反相色谱法分子排阻色谱法气相色谱法（GC）薄层色谱法（TLC）Ⅲ对照品标准Ⅳ高效液相色谱法测定原料药和制剂的验证参数准确度检测限和定量限线性精密度重现性进样重现性分析重现性2、中间精密度3、再现性E、范围F、回收率G、耐用性H、样品溶液稳定性I、专属性/选择性J、系统适应性试验1.容量因子2、进样重现性3、相对保留值4、分离度5、拖尾因子6、理论塔板数K、试验注意事项Ⅴ、评价和结论Ⅵ、致谢Ⅶ、参考文献指导原则综述高效液相色谱法验证指南简介The purpose of this technical review guide is to present the issues to consider when evaluating chromatographic test methods from a regulatory perspective. The document discusses the points to note and weaknesses of chromatography so that CDER reviewers can ensure that the methods performance claims are properly evaluated, and that sufficient information is available for the field chemist to assess the method. Analytical terms, as defined by the International Conference of Harmonization (ICH), 1993, have been incorporated in this guide.本指南旨在为在评估色谱分析方法时提供一个文件以供参考。这份指南主要讨论色谱法的一些注意点和不足之处，以便于CDER审评人员能正确评估文件中色谱法的性能阐述，也能给一些化学工作者提供一些色谱法相关信息。1993年ICH定义的分析专用术语在这里也有具体的介绍。Chromatographic methods are commonly used for the quantitative and qualitative analysis of raw materials, drug substances, drug products and compounds in biological fluids. The components monitored include chiral or achiral drug, process impurities, residual solvents, excipients such as preservatives, degradation products, extractables and leachables from container and closure or manufacturing process, pesticide in drug product from plant origin, and metabolites.色谱法常用于原材料、药用原料、药用制剂、生物制品的定量和定性的检测。色谱法可以具体运用于检测手性药物或者非手性药物，工艺杂质，残留溶剂、辅料例如防腐剂，降解产物，提取物，滤液，植物提取物中残留的杀虫剂和代谢产物。The objective of a test method is to generate reliable and accurate data regardless of whether it is for acceptance, release, stability or pharmacokinetics study. Data are generated for the qualitative and quantitative testing during development and postapproval of the drug products. The testing includes the acceptance of raw materials, release of the drug substances and products, in-process testing for quality assurance, and establishment of the expiration dating period.色谱法检测的目