ValidationProtocol驗證方案VAPNumber：VAP-OV-001Version版本：00ValidationProtocolforCleaningMethodforApparatusinLaboratory實驗室器具清洗方法驗證方案EffectiveDate生效日期：PagePAGE4/10 ValidationProtocolforCleaningMethodforApparatusinLaboratory實驗室器具清洗方法驗證方案DistributionQC分發質量控制部Writtenby：QC撰寫人Department（部門）華曉維Xiaowei.HuaDate（日期）Reviewedby：QC復核人Department（部門）安永宏SimonAnDate（日期）Approvedby：QAValidation批準人Department（部門）郭玉林牛莉珣YulinLisaGuo.NiuDate（日期）Approvedby：QA批準人Department（部門）江煥朝HuanchaoJiangDate（日期）TableofContent目錄Objective目的Scope范圍Reference參考文件Description描述Responsibilities職責Definition定義StandardOperatingProcedure(SOP)andTrainingProofQualification標準操作規程和培訓證明的確認Procedure程序UseSystemconfigurationsandcleaningagents系統配置和相關清潔劑CommonlyusedapparatuscleaningDifficultiesandeasyofanalysis常用器具清洗難易程度分析Laboratorytestsample實驗室目前日常檢測樣品Pollutionmethod污染方法CleaningMethod清洗方法Testmethodsandresults檢測方法和結果。VisualTest目測TOCTestTOC測試ConductivityTest電導率測試Deviation偏差Attachment附件RevisionHistory修訂歷史Objective目的ThisvalidationprotocolintendstodemonstratethattheSOP-01-022/01<WashingandDryingProcedureforGlassware>inQCLabiscorrectandeffectiveinPuraCaplaboratory.通過對普克QC實驗室的SOP-01-022/01《玻璃儀器的洗滌和干燥規程》草案進行驗證，證明此方法正確、有效。Scope范圍ThisprotocolappliestoSOP-01-022/01<WashingandDryingProcedureforGlassware>validationbyQCpersonalinPuracap.該方案適用于普克QC人員SOP-01-022/01《玻璃儀器的洗滌和干燥規程》草案的驗證程序。Reference參考文件USP現行版CurrentUSPSOP-01-022/01<WashingandDryingProcedureforGlassware>SOP-01-022/01《玻璃儀器的洗滌和干燥規程》草案TP-01-101/00<PurifiedwaterTestingMethod>TP-01-101/00《純化水檢測方法》Description描述The5affirmedglasswaresandsamplesinQCLabarepollutedbymethodunder8.3item.ThenwecleanthembySOP-01-022/01<WashingandDryingProceduresforGlassware>.TestwithVisualTest,TOCtestConductivityTest.Alltheresultsshouldbegoodtoensurethattheglasswaresarecleanedwellandtherearenononesampleresidual.實驗室中使用的器皿，在8.2項下確認的5種器皿和樣品，用8.3項下的方法污染器皿，按SOP-01-022/01《玻璃儀器的洗滌和干燥規程》草案清潔，用目測、TOC測試、電導率測試3種方法測試，結果要同時滿足這3種方法測試，以確認實驗室器皿中的樣品被清洗干凈，確保實驗室測試時器皿中無其它物質污染。Responsibility職責QualityControl質量控制部Draftandexecutethisdocument.起草和執行本方案.Reviewtheprotocolpriortoexecution在執行前審核本方案及報告。Handleprotocoldeviationsandprovideresolutions.處理和解決方案中出現的偏差。QualityAssurance質量保證部Approvetheprotocolpriortoexecution.在執行前審核本方案及報告。Reviewandapprovetheprotocoldeviationsandtheirresolutions.審核和批準方案的偏差及其解決辦法。Reviewandapprovereports.審核和批準報告。Description定義:N/AStandardOperatingProcedure(SOP)/SpecificationandTrainingProofQualification標準操作規程和培訓證明確認AcceptanceCriteria接受標準：TheinvolvedSOP-01-022/01<WashingandDryingProcedureforGlassware>shallbeapprovedandtheversioniscurrent，,DocumentedevidenceshallbeprovidedtoshowthatallinvolvedoperatorandtestingpersonnelaretrainedfortheseSOPs.Cleaningmethodforapparatusinlaboratoryhasbeenapproved.測試SOP-01-022/01《玻璃儀器的洗滌和干燥規程》已批準并且版本為現行版本,有文件證明所有相關的測試人員已經過培訓,實驗室器具清洗方法已經批準。確認：VerifythattherequiredSOPshasbeenapprovedandrelevantpersonnelreceivedpropertraining.檢查要求的SOP和質量標準已批準且相關人員的培訓已經完成。SOPorSpecificationTitleSOP或質量標準題目Doc.No./VersionNo.文件編號/版本號SOPUp-to-dateSOP現行版本TrainingProven培訓紀錄Sign/Date簽名/日期<WashingandDryingProcedureforGlassware>《玻璃儀器的洗滌和干燥規程》草案SOP-01-022/01□Yes□No□Yes□No<純化水檢測方法><PurifiedwaterTestingMethod>TP-01-101□Yes□No□Yes□NoProcedure程序ThisvalidationincludethefollowingSubproject本次驗證內容包括：Systemconfigurationsandcleaningagents系統配置和相關清潔劑CommonlyusedapparatuscleaningDifficultiesandeasyofanalysis常用器具清洗難易程度分析；Laboratorytestsample實驗室目前日常檢測樣品；Pollutionmethod污染方法Cleaningmethod清洗方法；Testmethodandresult檢測方法和結果。Testsystemconfigurationsandcleaningagents測試系統配置和相關清潔劑Testsystemconfigurations測試系統配置Testingmethod測試方法Name儀器名稱Model型號InstrumentcalibrationExpires儀器校正有效期TrainingProven培訓紀錄Sign/Date簽名/日期Visual目測N/AN/AN/AN/ATOCTOC總有機碳檢測儀□Yes□NoConductivity電導率Conductivitymeter電導率儀□Yes□NoCleaningAgents清潔劑Name名稱Lot批號Sources來源CIP100Water純化水CommonlyusedapparatuscleaningDifficultiesandeasyofanalysis常用器具清洗難易程度分析Cleaningobjects清洗對象Verifytestingapparatus.ApparatusthatwillbecleanedwithSOP-01-022/01<WashingandDryingProcedureforGlassware>areincludedinthefollowingform.Butthisvalidationwillselect5apparatuswhicharehardesttocleaned.Resultwillbefilledinthefollowingform.確認測試用的器皿，本表中列出本實驗室中將用SOP-01-022/01《玻璃儀器的洗滌和干燥規程》草案清洗的器皿，但本次驗證將從中挑選其中最難清潔的5種有代表性的器皿來運行本次驗證，結果填寫在下表中。Name名稱Standard規格MaterialQuality材質CleaingMethod清潔方法AnalysisCleanDegree清潔程度分析StandardforValidation(5apparatuswhicharehardesttoclean)選取驗證的規格(最難清潔的5種器皿)VolumatricFlask容量瓶ErlenmeyerFlask錐形瓶Sucker吸管Pipet移液管Burette滴定管Beaker燒杯Funnel漏斗TestTubewithStopper帶塞試管Pycnometer比重瓶WeighingBottle稱量瓶Flask燒瓶ColorimetricTube比色管Laboratorytestsample實驗室日常檢測樣品Select2or3kindsofsamplewhicharehardesttodissolveinwaterandCIP100(2%~5%)toverify.AccordingtoexcipientandAPI,solubilityinwaterandCIP100(2%~5%).Resultisfilledinthefollowingform.實驗室中經常檢測的輔料、API，根據其在水中及CIP100(2%~5%)中的溶解程度，分別選取在水中及CIP100(2%~5%)中最難溶解的2-3種樣品進行驗證，結果填寫在下表中。Name名稱Solubility溶解性質Water水中CIP100(2%~5%)中ExcipientsGelatin明膠Sorbitol山梨醇Glycerol甘油PEG400PropyleneGlycol丙二醇Povidone聚維酮PotassiumHydroxide氫氧化鉀PeppermintOil薄荷油SorbitolSolution山梨糖醇溶液AnhydrousSodiumCitrate無水檸檬酸鈉APIAcetaminophen對乙酰氨基酚DiphenhydramineHydrochloride鹽酸苯海拉明DocusateSodium多庫酯鈉Phenylephrine去氧腎上腺素DoxylamineSuccinate琥珀酸多西拉敏Dextromethorphan右美沙芬Benzonatate苯佐那酯Ibuprofen布洛芬Simethicone二甲基硅油Remark備注上面列出的樣品使用量均為0.1g，溶解體積分別為10ml、50ml、100ml，結果為易溶解、溶解、較難溶。其中明膠需加熱溶解。Applicationamountis0.1g.Dissolvevolumeare10ml,50ml,100mlrespsctively.Resultdescribeaseasilysoluble,soluble,difficulttodissolve.Gelatinshoulddissolvebyheating.Result結果通過以上溶解性對比研究，選擇、、、、為本次驗證中所需的最難溶解的樣品Comparetheabovesolubility.Select、、、、astherequiredsample.Pollutionmethod器皿污染方法OutwellDiscardtheresidueinapparatusaftertestingsample.Prepareaninitialconcentrationofsamplesolution.Soaktheapparatuswhichneedtoverifyinthesolutionfor10minutesorsuitabletime.Initialconcentrationofsolutionsareisasfollowingform.實驗室日常檢測完樣品后，將其所用的器皿殘留物倒掉，或將樣品配制成日常檢測首次濃度的溶液，將待驗證的器皿浸泡在其中10分鐘或適宜時間。首次濃度的溶液見下表。ApparatusName器皿名稱SampleName樣品名稱Firstpreparationconcetration首次配置濃度CleaningMethod清洗方法Cleanuptheapparatuspollutedbyabovemethodabove.CleaningmethodseefollowSOP-01-022/00<WashingandDryingProcedureforApparatus>draft.將殘留有8.3所述待驗證器皿清洗干凈，清洗方法見SOP-01-022/00《玻璃器皿的洗滌與干燥規程》草案。Testmethodandresult檢測方法和結果visualtest目測Method:Cleantheapparatusselectedby8.2.1accordingtoSOP-01-022/00<WashingandDryingProcedureforApparatus>draft.Thennumberthem.Visualthecleaningresult.ReservethelastwashingwaterforTOCtestin8.5.2andConductivityTestin8.5.3.Non-conformitywaterItwillnotconductTOCtestandConductivitytestifitdon’tpassthevisualtest.Theresultofvisualtestwillberecordedintheattachment9.3VAP-OV-001-A01.方法：將裝有按8.2.1選取樣品的器皿，按SOP-01-022/00《玻璃器皿的洗滌與干燥規程》草案中的方法清洗后編號，目測清洗后的清潔結果，保留最后一次清洗水，作為8.5.2TOC測試和8.5.3電導率測試。目測不合格的不能進行8.5.2TOC測試和8.5.3電導率測試。目測記錄在附件9.3VAP-OV-001-A01。Acceptancecriteria:Allapparatusshouldbenotgreasyandwithoutdroplet(Thewatershouldcomeoutinstrandswheninvertthecleanedapparatus.)接受標準：所有的器皿均應該無油膩，不掛水珠（洗凈的器皿倒置時，水成股流下，不掛壁）TOCTestTOC測試Method:Testthelastwashingwaterin8.5.1withTOC.SeeTP-00-031<TOCTestMethod>.Recordtheresultin9.4VAP-OV-001-A02.方法：取8.5.1項下的最后一次清洗水，檢測總有機碳，見TP-00-031《總有機碳測定法》。記錄在9.4VAP-OV-001-A02。AcceptanceCriteria:≤500ppb接受標準：≤500ppbConductivityTest電導率測試Method:Testthelastwashingwaterin8.5.1withconductivitymater.SeeTP-00-030<ConductivityTestingMethod>.Recordtheresultin9.5VAP-OV-001-A03.方法：取8.5.1項下的最后一次清洗水，檢測電導率，見TP-00-030《電導率測定法》。記錄在9.5VAP-OV-001-A03。AcceptanceCriteria:≤1.3μs/cm接受標準：≤1.3μs/cmDeviation偏差Anydeviationfromthisprotocolshouldbeproperlydocumented.tThereasonandcorrectiveactionshouldbedescribedinattachmentVAP-OV-001-A04DeviationLog針對該方案的任何偏差都應準確記錄,并在附件VAP-OV-001-A04《偏差記錄》中描述糾正措施及解決辦法。Attachment附表VAP-OV-073-A01VisualResults目測結果VAP-OV-073-A02TOCTestResultsTOC測試結果VAP-OV-073-A03ConductivityTestResults電導率測試結果VAP-OV-073-A04DeviationLog偏差記錄RevisionHistory修訂歷史Version版本Date日期DescriptionofChange變更描述002013..0506.1603NewVisualResults目測結果EffectiveDate生效日期DocumentNumber:VAP-O