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1、理想的實驗室操作(下),Analytical Method 分析方法Transfer, Verification, and Validation转移、确认和验证,Method Transfer方法转移,The process to establish documented evidence that the analytical method works as well in the receiving laboratory as in the originators laboratory, or the transferring laboratory, is called Analytica
2、l method transfer.用文件化的证明分析方法在接受实验室和原始实验室或者转移实验室一致的程序叫做方法转移,Method Transfer方法转移,Regulatory testing requires that a transfer of analytical methodology from research & development (R&D) to quality control (QC), contract (e.g. CRO), or process laboratory is performed to ensure and certify that other la
3、boratories are qualified to execute the method.法规要求从研发到QC，合约实验室，或者中控实验室的分析方法转移是为了确保和证明这些实验室有资质执行这个分析方法,Method Transfer方法转移, Original laboratory provides a method validation report to receiving laboratory.原始实验室提供给接收实验室一份方法验证报告。 After reading the report, the receiving lab writes a “Report Summary” and
4、 a “Method Transfer Protocol”.收到报告后，接收实验室写一份“报告总结”和“方法转移方案” Then execute the transferring work.然后执行方法转移工作。 Finally, document a “Method Transfer Report”.最后，形成一份“方法转移报告”文件。,Method Transfer方法转移,Review the validation report from originating laboratory回顾原始实验室提供的验证报告 Assay conditions 含量条件 Calculations 计算
5、System suitability 系统适用性 Receiving laboratory should perform the method接收实验室应按照分析方法执行。 To determine whether there are differences and gaps in documentation确认文件中是否存在差异和差别。,Method Transfer方法转移, Assess a subset of validation parameters 评估验证参数 Equivalence Testing 等价性测试 Precision and Accuracy 精密度和准确度 Key
6、 Attributes 关键的属性 Precision and Accuracy 精密度和准确度 LOD/LOQ 检测限和定量限 Identity 鉴别 Linearity 线性,Method Transfer方法转移,Typical Transfer should include: 典型的方法转移应该包括： More than one lot of testing materials 超过一批产品的检测 Reference Standard(s) 工作标准品 Samples 样品 Forced Degradation (Stress) Samples 强制降解样品 Typically the
7、 originating lab will prepare initialsample to be tested at both laboratories通常原始实验室会提供初始的样品供两个实验室检测 One analyst at the originating lab and multipleanalysts in the receiving lab.原始实验室的一个分析员和接收实验室的多个分析员,Method Transfer方法转移,Training of Analysts 分析员的培训 Training at originating laboratory 在原始实验室的培训 Revie
8、w of relevant SOPs 回顾相关的SOPs Observation of test procedures 观察测试程序 Performing test procedures 执行测试程序 Evaluate 评估 Reference Standard 工作标准品 Chemicals, Reagents 化学品，试剂 Solvents 溶剂,Points to consider需要考虑的要点,Equipment 仪器设备 Available? 是否可用？ Same Manufacturer? 是否同一生产商？ Calibrated or Qualified prior to use?
9、 使用前是否校验或确认 Gradient HPLC 梯度HPLC Dwell volume correction may have to be performed 需对死体积进行校正,Method Transfer Protocol方法转移方案,Test Method 测试方法 Parameters being assessed 需要评估的参数 Sample/Reagent preparations 样品和试剂准备 Instrument/Equipment/Apparatus 仪器设备 Performance Parameters 性能参数 Different analyst on diffe
10、rent days 不同天不同分析员 Predefined Acceptance Criteria 预先定好的可接受标准 Statistical Analysis 数据分析,Points to consider考虑的重点,Some minimal revalidation should be performed by the receiving laboratory:接收实验室最少应该重新验证的内容： Linearity 线性 LOD 检测限 LOQ 定量限 Recovery 回收率,Method Transfer Report方法转移报告,Include representative and
11、/or full data sets包括有代表性的或者全套数据： Chromatograms 色谱图 Standard Curves 标准曲线 Tabular Data 数据列表 Deviations 偏差 Statistical Analysis 数据分析 Conclusion 结论,Method Transfer Report方法转移报告,Follow the regulation requirements:遵循下列要求： Retain the testing articles保留测试记录 Retain the testing raw data保留测试原始数据 Verify the res
12、ults by second person第二个人对数据进行复核 Review and Sign by laboratory management实验室管理人员审核并且签名,Validation or Verification验证和确认,Analytical Methods described in 21 CFR 194(a)(2) “current version of USPNF, AOAC International Books of Methods, and methods detailed in an approved regulatoryapplications (NDA or ANDA) ” are not required to validate the accuracy and reliability of these methods, but need toverify their suitability under actual conditions of use.在21CFR 194（a）（2）描述：如果是USP现行版本的方法，或者是分析化学师协会（AOAC） 国际卷的方法，或是在已经批准过的（NDA或者ANDA）申请中的方法不要求确认这些方法的准确度和可靠性，但是需要确认在实际测试条件下的系统适用性。,
