USP〈1225〉药典规程的验证(中英文对照).pdf

VALIDATION OF COMPENDIAL PROCEDURES 药典药典规程规程的验证的验证 Test procedures for assessment of the quality levels of pharmaceutical articles are subject to various requirements.According to Section 501 of the Federal Food,Drug,and Cosmetic Act,assays and specifications in monographs of the United States Pharmacopeia and the National Formulary constitute legal standards.The Current Good Manufacturing Practice regulations 21 CFR 211.194(a)require that test methods,which are used for assessing compliance of pharmaceutical articles with established specifications,must meet proper standards of accuracy and reliability.Also,according to these regulations 21 CFR 211.194(a)(2),users of analytical methods described in USP-NF are not required to validate the accuracy and reliability of these methods,but merely verify their suitability under actual conditions of use.Recognizing the legal status of USP and NF standards,it is essential,therefore,that proposal for adoption of new or revised compendial analytical procedures be supported by sufficient laboratory data to document their validity.用于评价药物质量水平的测试规程受到多种要求的影响。根据联邦食品、药物、化妆品法案501 款，在美国药典和国家处方集的各论中的含量测定和质量标准构成了法定标准。现行药品优良生产规范【21 CFR 211.194(a)】要求，用于评价药物与既有质量标准之间的符合性的分析规程必须在准确度和可靠性方面达到适当的标准。并且根据这些法规【21 CFR 211.194(a)(2)】，在 USP-NF 中描述的分析规程的使用者无需验证这些规程的准确度和可靠性，而仅需确认其在实际使用条件下的适用性。认识到 USP 和 NF 标准的法律地位，因此，提议采纳新的或更改过的药典分析规程时，以充分的实验室数据作为支持，以记录其有效性，成为基本要求。The text of this information chapter harmonizes,to the extent possible,with the Tripartite International Conference on Harmonization(ICH)documents Validation of Analytical Procedures and the Methodology extension text,which are concerned with analytical procedures included as part of registration applications submitted within the EC,Japan,and the USA.本信息章节的内容尽可能地与三方国际协调会议（ICH）文件分析规程的验证和方法学的延伸内容保持一致，ICH 的内容关注的是作为在欧盟、日本、美国提交注册申请的一部分的分析规程。SUBMISSIONS TO THE COMPENDIA 向药典提交向药典提交的文件的文件 Submissions to the compendia for new or revised analytical procedures should contain sufficient information to enable members of the USP Council of Experts and its Expert Committees to evaluate the relative merit of proposed procedures.In most cases,evaluations involve assessment of the clarity and completeness of the description of the analytical procedures,determination of the need for the procedures,and documentation that they have been appropriately validated.Information may vary depending upon the type of method involved.However,in most cases a submission will consist of the following sections.向药典提交关于新的或更改过的分析规程的文件应该包括充足的信息，以使 USP 专家大会和其专家委员会能够评估拟议规程的相对优势。在大多数情况下，这些评估涉及对分析规程描述的清楚和完整程度的评价，对规程的需求的确定，以及它们已经进行了适当验证的记录文件。这些信息可以根据所涉及规程的种类而变化。但是，在大多数情况下，提交的文件将有下面的章节组成。Rationale-This section should identify the need for the procedure and describe the capability of the specific procedure proposed and why it is preferred over other types of determinations.For revised procedures,a comparison should be provided of limitations of the current compendial procedure and advantages offered by the proposed procedure.基本原理基本原理-此部分应该辨明对于该规程的需求，并描述具体拟议中规程的能力，以及其为什么优于其他种类检测。对于更改的规程，应该提供对当前药典规程之缺陷与拟议中规程之优势的比较。Proposed Analytical Procedure-This section should contain a complete description of the analytical procedure sufficiently detailed to enable persons“skilled in the art”to replicate it.The write-up should include all important operational parameters and specific instructions such as preparation of reagents,performance of system suitability tests,description of blanks used,precautions,and explicit formulas for calculation of test results.拟议的分析拟议的分析规程规程-此部分包含对该分析规程的完整描述，应足够具体以便能让业内技术熟练的人重复它。文章应该包括所有重要的操作参数和具体的指令，例如试剂制备、系统适用性测试表现、所使用空白对照的描述、预防措施、用于计算测试结果明确公式。Data Element-This section should provide thorough and complete documentation of the validation of the analytical procedure.It should include summaries of experimental data and calculations substantiating each of the applicable analytical performance characteristics.These characteristics are described in the following section.数据要素数据要素-此部分应该提供完全彻底的分析规程验证记录文件。其应该包括对于证明每一个实用工作特性的实验数据和计算的总结。这些特性在下面的部分描述。VALIDATION 验证验证 Validation of an analytical procedure is the process by which it is established,by laboratory studies,that the performance characteristics of the procedure meet the requirements for the intended analytical applications.Typical analytical performance characteristics that should be considered in the validation of the types of procedures described in this document are listed in Table 1.Because opinions may differ with respect to terminology and use,each of the performance characteristics is defined in the next section of this chapter,along with a delineation of a typical method or methods by which it may be measured.分析规程的验证是，通过实验室研究，确定该规程的工作特性达到了预定分析用途要求的过程。在此文件中所描述的规程种类的验证中，应当考虑的常见分析工作特性在表1 中列出。因为对于术语和使用的意见可能不同，在此通则的下个部分定义了每个工作性能，以及可以对其进行测量的常用的一个或几个方法的描绘。Table 1.Typical Analytical Characteristics Used in Method Validation 表表 1.在方法验证中使用的常用分析特性在方法验证中使用的常用分析特性 Accuracy 准确度 Precision 精密度 Specificity 专属性 Detection Limit