美国药典检验方法确认

1、Verification ：确认。针对使用法定方法 (注意: 需要严格遵守方法要求， 参数, 试剂, 标准品, 步骤等等), 需 要在目前实验室的条件下确认是否可以获得可靠结果 . 不一定是全部项目的验证， FDA 针对常州 SPL 肝素 钠的警告信中就有关于方法确认的内容 . 可以参考。 VERIFICATION OF COMPENDIAL PROCEDURES 药典规程的确认 The intent of this chapter is to provide general information on the verification of compendial procedures th

2、at are being performed for the first time to yield acceptable results utilizing the personnel, equipment, and reagents available. This chapter is not intended for retroactive application to already successfully established laboratory procedures. The chapter Validation of Compendial Procedures provid

3、es general information on characteristics that should be considered for various test categories and on the documentation that should accompany analytical procedures submitted for inclusion in USP-NF. Verification consists of assessing selected analytical performance characteristics, such as those th

4、at are described in chapter , to generate appropriate, relevant data rather than repeating the validation process. 本章节的目的是提供关于药典规程确认的信息，这些规程是第一次执行，利用可用的人员、设备和 试剂，来生成可接受的结果。本章节不是为了对已经成功确立的实验室规程进行追溯操作。通则药典规程 的验证 提供了关于不同测试种类应当考虑的特性， 以及应当生成文件连同分析操作规程一起提交给 相关部门以便列入 USP-NF (美国药典 /国家处方集)。确认包括评估选定的分析工作特性，例如

5、那些 在通则 中描述的，以生成适合、相关的数据，而不是重复验证程序。 Users of compendial analytical procedures are not required to validate these procedures when first used in their laboratories, but documented evidence of suitability should be established under actual conditions of use. In the United States, this requirement is est

6、ablished in 21 CFR 211.194(a)(2) of the current Good Manufacturing Practice regulations, which states that the“ suitability of all testing methods used shall be verified under actual conditions of use.” 药典分析规程的使用者无需于规程在实验室中初次使用时验证这些规程，但是关于在实际使用条件 下的适用性的证据应当以文件形式记录。在美国，这些要求在现行药品生产质量管理规范的 21 CFR 211.1

7、94(a)(2) 中有明确规定，文件声明 “所有测试方法在实际使用条件下的适用性应当被确认。 ” Verification of microbial procedures is not covered in this chapter because it is covered in USP general chapters Antimicrobial Effectiveness , Microbiological Examination of Non-sterile Products: Microbial Enumeration Tests , Microbiological Examinat

8、ion of Non-sterile products: Tests for Specified Microorganisms, Sterile Tests , and Validation of Microbial Recovery from Pharmaceutical Articles. 微生物规程的确认方法不在此章节内， 因为其由以下 USP 通则涵盖： 抗菌效力 、非无菌产品的 微生物学检查：微生物计数测试 、非无菌产品的微生物学检查：规定微生物的测试 、无菌测试 、药物微生物回收的验证 VARIFICATION PROCESS 确认程序 Users should have the

9、appropriate experience, knowledge, and training to understand and be able to perform the compendial procedure as written. Verification should be conducted by the user such that the results will provide confidence that the compendial procedure will perform suitably as intended. 使用者应该有适当的经验、知识以及培训，以便能

10、够理解和执行药典规程。确认应当由使用者进行， 确认结果将提供该药典规程可以如预期般适当合理执行的证据。 If the verification of the compendial procedure is not successful, and assistance from USP staff has not resolved the problem, it may be concluded that the procedure may not be suitable for use with the article being tested in that laboratory. It m

11、ay then be necessary to develop and validate an alternate procedure as allowed in the General Notices. The alternate procedure may be submitted to USP, along with the appropriate data, to support a proposal for inclusion or replacement of the current compendial procedure. 如果药典规程的确认失败，并且 USP 员工的协助也未能

12、解决问题，则可断定此规程不适合在此实验 室用于该供试物品。因此，可能必须按照凡例中所说开发和验证替代规程。此替代规程连同适当的数据提 交给 USP ，以支持将其加入或取代当前药典规程的方案。 VERFICATION REQUIREMENTS 确认要求 Verification requirements should be based on an assessment of the complexity of both the procedure and the material to which the procedure is applied. Although complete reval

13、idation of a compendial method is not required to verify the suitability of the method under actual conditions of use, some of the analytical performance characteristics listed in chapter , Table 2, may be used for the verification process. Only those characteristics that are considered to be approp

14、riate for the verification of the particular method need to be evaluated. The degree and extent of the verification process may depend on the level of training and experience of the user, on the type of procedure and its associated equipment or instrumentation, on the specific procedural steps, and

15、on which article(s) are being tested. 确认要求所进行的评估应该基于此规程和要应用此规程的物质的复杂性。虽然无需对药典方法进行 完整的再验证以确认该方法在实际使用条件下的适用性， 但是可以将在通则 表 2 中列出的一些分析 工作特性用于确认程序。只有当被认为适合于特定方法的确认时，那些特性才需要被评估。确认程序的程 度与层次取决于使用者的培训和经验水平、规程种类和其相关设备与仪器、具体的规程步骤、供试物质。 As an example, an assessment of specificity is a key parameter in verifying

16、that a compendial procedure is suitable for use in assaying drug substances and drug products. For instance, acceptable specificity for a chromatographic method may be verified by conformance with system suitability resolution requirements (if specified in the method). However, drug substances from

17、different suppliers may have different impurity profiles that are not addressed by the compendial test procedure. Similarly, the excipients in a drug product can vary widely among manufacturers and may have the potential to directly interfere with the procedure or cause the formation of impurities t

18、hat not addressed by the compendial procedure. In addition, drug products containing different excipients, antioxidants, buffers, or container extractives, may potentially interfere with the compendial procedure. In these cases, a more thorough assessment of specificity may be required to demonstrat

19、e suitability of the method for the particular drug substance or product. Other analytical performance characteristics such as an assessment of the limit of detection or quantitation and precision for impurities procedures may be useful to demonstrate the suitability of the compendial method under a

20、ctual conditions of use. 作为范例，在证明某个药典规程适用于对原料药和成药进行分析时，专属性的评估是关键参数。例 如，色谱法中可接受的专属性可以通过与系统适用性的分离度要求（如果在方法中做出了规定）的符合性 来证实。但是，来自不同供应商的原料药可能有不同的杂质情况，并且没有被药典测试规程所解决。相似 的是，成药中的辅料在不同生产商之间可能大大不同，并可能有药典规程尚未解决的杂质。此外，含有不 同的辅料、抗氧化剂、缓冲液、容器提出物的成药可能会潜在地干扰药典规程。对于这样的情况，可能需 要对专属性进行更加全面的评估，以证明该方法对于特定原料药或成药的专属性。其他分析工作特性，例 如对于杂质规程的检测限度、定量限度、精密度的评估，可以用于论证在实际使用条件下药典方法的适用 性。 Verification is not required for basic compendial test procedures that are routinely performed unless there is an indication tha