新药分析方法的建立与验证

1、分析方法的建立与验证上海浦融生物科技有限公司上海浦融生物科技有限公司 ChamQuestChamQuest1上上海海浦浦融融ChamQuestChamQuest分析方法的建立与验证0. 引言1. 分析方法在药品开发中的应用2. 分析方法开发的基本问题3. 分析方法的验证与转移20. 引言上海浦融生物科技有限公司上海浦融生物科技有限公司 ChamQuestChamQuest3上上海海浦浦融融ChamQuestChamQuest药物质量体系Investigational ProductsPharmaceutical DevelopmentTechnology TransferCommercial ManufacturingProduct DiscontinuationGMPManagement ResponsibilityKnowledge ManagementQuality Risk ManagementProcess Performance Imp:RT-SL-2SL) 含量范围的下限 含量范围的中间 含量范围的上限 2)对于控制样品记录下列内容: 将使用哪种类型的样品及原因. 如何制

2、备控制样品 验收标准 1)单个加样回收率:96-104% 2)每个水平的平均回收率: 97-103% 3)单个控制样品的回收率: 理论值的98-102% 4)对于精密度, 整体的 RSD (n=9): ) 注射6针中间含量的溶液 (活性药物 + 杂质) 验收标准 1)峰响应值的 RSD % : 2% 2)保留时间（RT）的RSD % : 5% 3)托尾因子: 0.5 T 2.5 4)分离度: 基线峰之间的分离度包括溶剂前沿, 通常应 1.5. 5)容量因子: 1.5 灵敏度样品 分离度样品87上上海海浦浦融融ChamQuestChamQuest测样顺序 系统适用性测定 洗脱 空白溶液/辅料 灵敏度样品测定 分离度样品测定 洗脱 线性测定 QC 样品 洗脱 样品 核对标准品88Method Transfer89上上海海浦浦融融ChamQuestChamQuestModel with General Timeline for Technology Transfer Phase IPhase IIA Clinical TrialsPhase III Clinical TrialsFiling

3、 and LaunchEarly Development Starting Point - (Sourcing Decision)Registration Batches (Phase III Clinical Trials)Pre-Validation (Final Scale-Up Activities)Validation*LaunchFilePAIFull DevelopmentEnd PointFiling and LaunchProcessOutputsDevelopment ActivitiesDevelopment ReportsPDIRTTPPTTSPIRPhase IIbTransfer Signoff AcceptanceAMTR (In-Process testing)Analytical Pre-TransferAnalytical Method Transfer AMTRMicro Method TransferMDDSMMTRADDSPTRTimeline for ActivityTTS Technology Transfer StrategyTTPP T

4、echnology Transfer Project PlanPIR Product Introduction ReportPDIR Pharmaceutical Development Interim ReportReport Name AbbreviationsADDS - Analytical Development Documentation SetAMTR Analytical Method Transfer ReportAMTR (In-Process Testing) Analytical Method Transfer Report for in-process testing transferPTR Product Transfer ReportMMTR Microbiological Method Transfer ReportMDDS Microbiological Development Documentation SetOngoing Activity (as required) *Validation may occur prior to regulator

5、y submission90上上海海浦浦融融ChamQuestChamQuestScope分析技术转移的任务 Different tasks part of the Analytical Technology Transfer are: analytical methods (分析方法) Specifications (规格) Stability (稳定性) reference materials (标准物) cleaning validation (清洁验证) release of registration and validation batches (注册批量和验证批量的释放) Knowledge (知识)91上上海海浦浦融融ChamQuestChamQuest方法转移过程 (JNJ)GATTATT Project PlanMethod DevelopmentAT Ring TestMethod ValidationDevelopment Document SetMethod TransferTransfer of OwnershipATT StrategyTechnology

6、Transfer Strategy PhaseDevelopment PhaseSite Transfer Phase92上上海海浦浦融融ChamQuestChamQuest方法转移过程(JNJ SOP) Phase I Preparation Id documentation, personnel from each lab Verify equipment equivalency Determine training requirement Determine testing requirement Generate protocol Approval protocol Phase II Execution Obtain test samples and standards Train receiving lab analysts Complete training document Perform equipment eq testing (if applicable) Perform transfer testing Review and approve data (each

7、lab individually) Generate summary report (receiving lab) 93上上海海浦浦融融ChamQuestChamQuest方法转移过程 Phase III Evaluation and Report Evaluate test results per acceptance criteria establshed in Transfer Protocol (Originating lab) Write final report (Originating lab) Review and approve final report94上上海海浦浦融融ChamQuestChamQuest方法转移计划书范例: A Release Rate Method Protocol Index 1.0 Scope 2.0 Attachments 3.0 Objective 4.0 Facilities 5.0 Location of Raw Data 6.0 Training 7.0 Equipment and Materials 8.0 Testing an

8、d Acceptance Criteria 9.0 Discussion and Conclusion 10.0 Reference Documents95上上海海浦浦融融ChamQuestChamQuest方法转移计划书范例:A Release Rate Method 7.1Drug release rate (AAM 1.810) Testing Samples will be tested in accordance with AAM 1.810. Both sending and receiving laboratories will perform testing as per the following plan. Both sending and receiving labs will each prepare 12 individual sample preparations for both strengths as per the method. The sending laboratory will use data previously generated fo

9、r the lot clearance. The receiving lab will summarize their results and send them to the transferring lab for evaluation against the acceptance criteria. Any deviations from the protocol must be reported to the transferring lab for evaluation and documented in the transfer report. All individual results must be reported in mg/cm2 to 3 decimal places (e.g. 0.152 mg/cm2). Means must be calculated on un- rounded results and must be reported to 3 decimal places. 96上上海海浦浦融融ChamQuestChamQuest方法转移计划书范例:A Release Rate Method System suitability requirements of the method must be achieved in both labs. The absolute difference in mean cumulative amounts released (mg/cm2) between both labs at each of the specified time intervals must be 5.0% of the label claim. The %RSD (n=24) of both labs results must be 10% for t

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