分析方法验证程序

1、分析方法验证程序 SOP 审核和批准 SOP Review and Approval 1.0 2.0 3.0 目的 Purpose 本规程的目的是为在 XXX 有限公司进行的验证研究制定一个程序，包括分析方法验证 过程，分析方法的确认，文件记录，审计，原始数据归档以及验证 / 确认文件放行。 范围 Scope 2.1 本标准操作程序适用于 XXX有限公司产品研发部门 GMP分析实验室， 采用色谱技术对最终成品和 API （如适用）进行的所有分析方法的验证 / 确认。 2.2 本标准操作程序也可作为 XXX 有限公司产品研发部门分析研发实验室， 采用其他分析技术进行其他任何方法验证 / 确认的参

2、考。 c. 职责 Responsibility 3.1 分析员 Analyst 3.1.1 负责准备验证方案 3.1.2 / of method validation / method 3.1.3 / 确认报告 Responsible for preparation of method validation report / method verification report 3.2 4.0 主管小组 / 指定人员 Group In-charge/ Designee 3.2.1 负责复核和审批验证方案 Responsible for review & approval of validati

3、on protocol 3.2.2 负责方法验证 / 确认活动的分配、监督以及验证 / 确认数据的复 核 Responsible for allotment & monitoring of method validation / verification activity and review of validation / verification data 3.2.3 负责验证报告 / 确认报告的复核和审批 Responsible for review & approval of validation report / verification report 3.3 质量保证 Qualit

4、y Assurance 3.3.1 负责验证报告 / 确认方案的复核和审批 protocol 3.3.2 负责验证报告 / report 3.4 注册 Regulatory 3.4.1 负验 / 案的复核 Responsible for review of 简写和定义 为了启动方法验证，相关人员或者指定人员应该起草验证方案。验证方案应该包含在 验证过程中所有需要研究的参数和接受标准。相关主管或者指定人员应该对验证方案进行 复核。 To initiate method validation, a validation protocol should be filled by the concer

5、ned person / designee. The validation protocol should contain all the parameters required to be studied during the validation along with acceptance criteria. Validation protocol should be checked by the concerned group head / designee. 备注：对于方法确认，不要求准备方案。 Note:There is no requirement to prepare any p

6、rotocol for method verification activity. 验证方案应该有 QA 给定的唯一编号。 The validation protocol should have a unique number given to it by the quality assurance. 5.1 5.2 5.3 5.4 5.5 QA 和注册(如适用)批准。 charge /designee followed by a representative of QA& Regulatory (if applicable). / 观 pH 测定)。 Validation be record

7、ed in laboratory note book (dedicated for validation only) against each approved validation notebook.Verification is not required for basic compendial test procedures that are routinely performed (e.g. loss on drying, residue on ignition, various wet chemical procedures such as acid value, and simpl

8、e instrumental determinations such as pH measurements). 在实验进行过程中或者实验完成后，来自方案的任何偏差应该被评估。任何来自方案 的增补或变更应该在验证方案的合适章节中提到。 During the execution of experimental work or after its completion, any deviation from the protocol should be justified. Any additions or changes from the protocol should be mentioned

9、under appropriate section in validation protocol. 如果在之后的时间里，发现批准的方案中有一些小的差异或错误，如印刷或输入错误， 主管或指定人员应该用“勘误表”说明并纠正这些错误。If at a later date minor discrepancies or errors are noticed in the approved validation protocol, such as typographical and transcriptional errors, an 5.6 ERRATUM stating these errors, a

10、long with the correction, should be prepared by the group in-charge/designee. 5.7 在验证研究过程中，如果需要做额外的一些实验 / 参数，但它们不是主验证方案的一 部分，就需要再产生一个补充方案（以及相应的编号），补充的实验将成为验证报告的一 部分。 During the course of validation studies, if any additional experiment / parameter needs to be done which is not part of the main valid

11、ation protocol, an addendum protocol （and corresponding number） need to be taken, if that additional experiment will be part of validation report. 备注：补充验证方案可在最终的验证报告批准前的任何时间产生。最终的验证报告应 包括来自于主验证方案和补充验证方案 （如果有 ） 的数据。 Note: Addendum validation protocol can be taken any time before the approval of final

12、 validation report. The final validation report should include the data generated against the main validation protocol and addendum 5.9 单个验证方案中的接受标准可参考附件 -A 中规定的接受标准，最终在批 准的验证方案中的规定接受标准将会取代SOP中规定的接受标准。 The acceptance criteria specified in appendix-A can be used as reference to define the acceptance

13、criteria in the individual validation protocol. Finally, the acceptance criteria specified in approved validation protocol will supersedes the acceptance criteria specified in this standard operating procedure. 5.10 在实验工作和计算完成后，分析员应该准备验证 / 确认报告草案。 On completion of the experimental work and calculati

14、ons, a draft validation report/ verification report should be prepared by analyst. 5.11 主管/ 指定人员以及之后的 QA ，应该从准确度和完整性角度审核验证/ 确 认报告草案和方法验证研究的原始记录。 The draft validation report / verification report and the raw data of the method validation studies should be reviewed for accuracy and adequacy by group-i

15、n-charge / designee, followed by quality assurance. 5.12 告。 5.13 分析部门主管 /QA/ 指定人员审批。 报告应该有 QA The report should by Head Analytical Research (or R&D) / Designee, Assurance / Designee. The validation report 5.14 The final copy of the report along with the raw data should be archived. The draft reports

16、hould not be retained. 5.15 如果在最终报告签署后，要求产生额外的数据而不是更新原来已经存在 的数据，应进行额外的实验工作，并准备一份原报告附录，放行额外产生的数据。 If at a later date additional data other than the already existing data is required to be generated, additional experimental work should be carried out and an addendum to the original validation report s

17、hould be prepared and issued. 5.16 如果报告批准后，发现一些小的差异和错误，如印刷或输入错误(不超 5 个或 过 5 个)，应准备“勘误表”说明和纠正这些错误。如果印刷或输入错误超过 者需要对一些现存数据的报告进行修正，那就需要准备和放行修订版本的报告或者补充报 告。 If at a later date minor discrepancies or errors are noticed in the approved reportreport, such as typographical and transcriptional errors (not mor

18、e than five in number), an ERRATA stating these errors, along with the correction, should be prepared. If the typographical and transcriptional errors are more than five or there is any modification in the reporting of an existing data, a revised v report or addendum report should be prepared and is

19、sued. 5.17 原报告修订的原因应该清晰地在修订的报告中阐述。修订报告和原始记 录应该交给 QA 审计。 The reason for revision of the original report should be clearly stated in the introduction of the revised report. The revised validation report and the raw data should be submitted to quality assurance for audit. 5.18 批准的报告，以及原始记录、补充文件、勘误表和升级版本，都应该归