<1225>V ALIDATION OF COMPENDIAL PROCEDURES
药典规程的验证
Test procedures for asssment 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 ud for asssing compliance of pharmaceutical articles with established specifications, must meet proper standards of accuracy and reliability. Also, according to the regulations [21 CFR 211.194(a)(2)], urs of analytical methods described in USP-NF are not required to validate the accuracy and reliability of the methods, but merely verify their suitability under actual conditions of u. Recognizing the legal status of USP and NF standards, it is esntial, therefore, that proposal for adoption of new or revid compendial analytical procedures be supported by sufficient laboratory data to document their validity.
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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 C
FR 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.
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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向药典提交的文件Submissions to the compendia for new or revid 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 propod procedures. In most cas, evaluations involve asssment of the clarity and completeness of the description of t当我们同在一起
he 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 cas a submission will consist of the following ctions.
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 ction should identify the need for the procedure and describe the capability of the specific procedure propod and why it is preferred over other types of determinations. For revid procedures, a comparison should be provided of limitations of the current compendial procedure and advantages offered by the propod procedure.
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。
Propod Analytical Procedure---This ction 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 ud, precautions, and explicit formulas for calculation of test results.
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拟议的分析规程----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。
难忘的节日Data Element----This ction 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. The characteristics are described in the following ction.
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。
V ALIDATION验证
鱼的特点Validation of an analytical procedure is the process by which it is established, by laboratory studies, t
hat 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. Becau opinions may differ with respect to terminology and u, each of the performance characteristics is defined in the next ction 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 Ud in Method Validation
表1. 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检测限度
Quantitation Limit定量限度
Linearity线性
Range范围
Robustness耐用性
In the ca of compendial procedures, revalidation may be necessary in the following cas: a submission to the USP of a revid analytical procedure; or the u of an established general procedure with a new product or raw material (e below in Data Elements Required for Validation). 对于药典规程，在下面的情况下可能必需在验证：向USP提交修改的分析规程；或将已确立的通用规程用于新产品或原料（见下面验证必需的数据要素）
The ICH documents give guidance on the necessity for revalidation in the following circumstances: changes in the synthesis of the drug substance; changes in the composition of the drug product; and changes in the analytical procedure.
ICH文件对于下列情况下再验证的必要性做出了指导：原料药合成中的变更；成药组成中的变更；以及分析规程中的变更。正方形简笔画
Analytical Performance Characteristics分析工作特性
ACCURACY准确度
Definition---- The accuracy of an analytical procedure is the cloness of test results obtained by that procedure to the true value. The accuracy of an analytical procedure should be established across its range.
定义----分析规程的准确度是由该规程得到的测试结果与真实值的接近程度。分析规程的准确度应该在其整个范围内得到确立。
Determination----In the ca of the assay of a drug substance, accuracy may be determined by application of the analytical procedure to an analyte to known purity (e.g., a Reference Standard) or by comparison of the results of the procedure with tho of a cond, well-characterized procedure,
the accuracy of which has been stated or defined.
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测定---- 对于原料药的含量测定，可以用该分析规程来分析已知纯度的被分析物（例如，某个标准物质），或将以此规程所得的结果与第二种、成熟的、已知准确度的规程所得的结果进行比较，以测定其精确性。
In the ca of the assay of a drug in a formulated product, accuracy may be determined by application of the analytical procedure to synthetic mixtures of the drug product components to which known amounts of analyte have been added within the range of the procedure. If it is not possible to obtain samples of all drug product components, it may be acceptable either to add known quantities of the analyte to the drug product (i.e., “to spike”) or to compare results with tho of a cond, well-characterized procedure, the accuracy of which has been stated or defined.
对于处方产品中某个药物的含量测定，以该分析规程来分析成药各组分的合成混合物，其中已经在这些组分的范围之内加入已知数量的待分析物。如果不可能得到成药的所有组分，也可以将已知数量的待分析物加入到该成药中（例如，“增敏”），或者将结果与用第二种、成熟的、已知准确度的规程得到的结果进行比较，
In the ca of quantitative analysis of impurities, accuracy should be assd on samples (of drug substance or drug product) spiked with known amount of impurities. Where it is not possible to obtai
n samples of certain impurities or degradation products, results should be compared with tho obtained by an independent procedure. In the abnce of other information, it may necessary to calculate the amount of an impurity bad on comparison of its respon to that of the drug substance; the ratio of the respon of equal amounts of the impurity and the drug substance (relative respon factor) should be ud if known.
对于杂质的定量分析，应使用以已知数量杂质增敏的样品来评估准确度。当不可能获得特定杂质或降解产物的样品时，应将结果与得自独立规程的的结果进行比较。在没有其他信息的情况下，可能必需通过将某种杂质的响应值与药物的响应值进行比较来计算杂质的数量；同等数量的杂质与药物的响应值的比值（相对响应因子），如果已知，则应使用。
Accuracy is calculated as the percentage of recovery by the assay of the known added amount of analyte in the sample, or as the difference between the mean and the accepted true value, together
