質(zhì)量控制概要中英文課件

ReviewofQualityControl

質(zhì)量控制概要Wewillcover(內(nèi)容)Terminology術(shù)語CharacteristicsofAnalyticalMethods分析方法特性TypesofQCsamplesandhowtheyrelatetothecharacteristicsQC樣品類型和特性1ReviewofQualityControl

質(zhì)量控DefinitionofQuality

質(zhì)量的定義Tomostoftheworld(普遍上)degreeofexcellence(優(yōu)異程度)TotheISOworld(在ISO領(lǐng)域)degreeofagreementbetweencharacteristicsandrequirements特性與要求的吻合程度Moreimportantly(更重要)toourclients?(對客戶)2DefinitionofQuality

質(zhì)量的定義ToQualityControlvs.QualityAssurance(質(zhì)量控制與質(zhì)量保證)Qualitycontrolisaseriesofmeasurementsusedtoassessthequalityoftheanalyticaldata質(zhì)量控制是一系列測量,以評價分析數(shù)據(jù)的質(zhì)量Howwellisthetestfulfilling

requirements?試驗滿足要求的程度如何?3QualityControlvs.QualityAsQualityControlvs.QualityAssurance(質(zhì)量控制與質(zhì)量保證)Qualityassuranceisamanagementplantoensuretheintegrityofdata(asystem)質(zhì)量保證是一種管理計劃,以確保數(shù)據(jù)的完整性(一種體系)Providesconfidencethatrequirementswillbefulfilled為要求是否得到滿足提供信心4QualityControlvs.QualityAsQualitiesofAnalyticalMethods

分析方法的質(zhì)量Accuracy(準(zhǔn)確度)Precision(精密度)Selectivity(選擇性)Sensitivity(靈敏度)Linearity(線性)Range(范圍)Robustness/Ruggedness(穩(wěn)健性/穩(wěn)度)5QualitiesofAnalyticalMethoAccuracy(準(zhǔn)確度)Degreeofagreementbetweenthe“true”valueandthemeasuredvalue(真值與測量值之間的一致程度)6Accuracy(準(zhǔn)確度)DegreeofagreemeAccuracy(準(zhǔn)確度)Whatisthe“true”value?(什么是真值)Theoretical(理論值)Consensus(公議值)Accepted/Assigned(可接受/賦值)7Accuracy(準(zhǔn)確度)7Accuracy(準(zhǔn)確度)Expressedas(表示為)theratiobetweentheassayedvalueandthe“true”value(%recovery)分析值與真值間的比(%回收率)thedifferencebetweentheassayandtheacceptedtruevalue(%Error)分析與可接受真值間的差(%誤差)8Accuracy(準(zhǔn)確度)Expressedas(表示Precision(精密度)Closenessofagreementbetweenmeasurements(測量間的一致程度)Repeatability(r)–sameconditions,shorttimeinterval(samerun)–shorttermprecision重復(fù)性(r)-相同條件下\短時間間隔-短期內(nèi)精密度Intermediateprecision–samelabdifferentday,analyst,instrument中間精密度-同一實驗室不同日期,分析人員,儀器Reproducibility(R)–agreementbetweenbatchesorbetweenlabs復(fù)現(xiàn)性?-批間或?qū)嶒炇议g的一致性9Precision(精密度)ClosenessofagrPrecision(精密度)ExpressedasStandardDeviation,RelativeStandardDeviationorRelativePercentDifference表示為標(biāo)準(zhǔn)偏差、相對標(biāo)準(zhǔn)偏差、相對百分差10Precision(精密度)ExpressedasStSensitivity（靈敏度）Degreeofresponsetoachangeinanalyteconcentration–resolution被分析物濃度變化的響應(yīng)變化程度-分辯率Lowestconcentrationthatcanbedistinguishedfrombackgroundnoise–detectionlimit能從背景噪音識別出的最低濃度-檢測限11Sensitivity（靈敏度）DegreeofrespSensitivity（靈敏度）Limitofdetectionvs.Limitofquantification（檢測限與定量限）Limitofdetection(LOD)isthelevelthatwecansaywhetherananalyteispresentornot檢測限是我們判斷被分析物是否存在的含量水平Limitofquantitation(LOQ)isthelevelthatwecanquantifytheanalytewithaspecifiedaccuracy(20%)定量限是我們按規(guī)定準(zhǔn)確度（20%）能對被分析物量化的含量水平12Sensitivity（靈敏度）LimitofdeteSelectivity（選擇性）Abilitytodetecttheanalyteinacomplexmatrix檢測復(fù)雜基體中被析物的能力Abilitytoexcludenon-analytespeciesfromsignal通過信號排除非被分析物的能力Usuallyinverselyrelatedtosensitivity通常與靈敏度成反比13Selectivity（選擇性）AbilitytodetLinearity（線性）Abilitytoproducearesponsethatisdirectlyproportionaltotheconcentrationoftheanalyte所產(chǎn)生的反應(yīng)與被分析物濃度成正比的能力Onlyholdstruewithinagivenrange只在給定范圍內(nèi)是真實的14Linearity（線性）AbilitytoproducLinearity（線性）Expressedascorrelationcoefficient(r)orcoefficientofdetermination(r2)表示為相關(guān)系數(shù)(r)或測定系數(shù)(r2)r2=ssxy2/ssxxssyy15Linearity（線性）ExpressedascorRange（范圍）Theintervalbetweenthehighestandlowestconcentrationforwhichthemethodhasshowntohavesuitablelevelsofaccuracy,precisionandlinearity.在方法具有適宜的準(zhǔn)確度、精密度和線性的條件下，最高和最低濃度范圍16Range（范圍）TheintervalbetweenRobustness（穩(wěn)健性）Abilityofmethodtobeunaffectedbysmallchangesinmethod(internal)conditions（方法不因條件的較小變化（內(nèi)部）而受影響的能力）Temperature（溫度）pHCompositionofmobilephase（流動相組成）Usefulwhenmethodmovesfromdevelopmenttoproduction（從方法開發(fā)到使用很有用）17Robustness（穩(wěn)健性）AbilityofmethRuggedness（穩(wěn)度）Abilityofmethodtobeunaffectedbyexternalconditions（方法不受外界條件影響的能力）Differentanalysts（不同的分析人員）Differentlaboratories（不同的實驗室）Differentreagentlots（不同批的試劑）Differentinstruments（不同的儀器）18Ruggedness（穩(wěn)度）AbilityofmethoRuggedness（穩(wěn)度）Usefulfortechnologytransfer（對技術(shù)推廣很有用）19Ruggedness（穩(wěn)度）UsefulfortechQualityControlMeasures

質(zhì)量控制手段Calibrationstandards（校準(zhǔn)標(biāo)準(zhǔn)）Blanks（空白）Recoverystudies（回收率研究）Precisionstudies（精密度研究）Sensitivitystudies（靈敏度研究）DetectionLimit（檢測限）Quantitationlimit（定量限）20QualityControlMeasures

質(zhì)量控制手

Calibration(校準(zhǔn))Directlyaffectsaccuracy(直接影響準(zhǔn)確度)Preparationofstandards(標(biāo)準(zhǔn)制備)Matrix(基體)Stability(穩(wěn)定性)Signaltype:peakarea,peakheight信號類型:峰面積,峰高21Calibration(校準(zhǔn))DirectlyaffeCalibration(校準(zhǔn))Calibrationcurves(校準(zhǔn)曲線)1storder–straightline(一級-直線)Quadratic–acceptablebutrequiresmorepoints(二次方程-可以接受,但需要更多點)Internalstandards(內(nèi)標(biāo))Refinescalibrationresponse(增強校準(zhǔn)響應(yīng))Addedtosamplesandstandards(加入樣品和標(biāo)準(zhǔn)中)Mustbehaveliketheanalyte(象被分析物一樣表現(xiàn))Cannotbeinsamples–rareelements,deuteratedcompounds(樣品中沒有-稀有元素,含重氘的化合物)22Calibration(校準(zhǔn))CalibrationcuCalibration(校準(zhǔn))Calibrationverification(校準(zhǔn)驗證)Repeatedcalibrationstandard重復(fù)校準(zhǔn)標(biāo)準(zhǔn)Intervalmaybeevery20samples(ICPMS)oronceeveryrun(GC-FID)間隔:20個樣品(ICPMS)每次(GC-FID)23Calibration(校準(zhǔn))CalibrationveBlanks(空白)Usedtomonitorcontamination(監(jiān)測污染)Reagentblanks(試劑空白)Instrumentblanks(儀器空白)Fieldblanks(場地空白)Tripblanks(路途空白)Procedural/methodblanks(程序/方法空白)Matrixblanks(基體空白)Others?(其它)24Blanks(空白)UsedtomonitorcontRecoveryStudies（回收率研究）Usedtomonitoraccuracy（監(jiān)測準(zhǔn)確度）Matrixspikes（基體加標(biāo)）Fortifiedblanks（增加加標(biāo)）Surrogates（替代）ReferenceMaterials（參考物質(zhì)）25RecoveryStudies（回收率研究）UsedtoMatrixSpikes（基體加標(biāo)）Knownamountofanalyteaddedtosample在樣品中加入已知量的被分析物Importantwithcomplexmatrix對復(fù)雜基體很重要Generallyaddedpriortoextractionprocess（通常在提取前加入）Sometimesdifficulttoknowamounttospikeaheadoftime（有時很難提前知道加標(biāo)量）26MatrixSpikes（基體加標(biāo)）KnownamounFortifiedBlanks（增強空白）Analytespikeintoreagentblank在試劑空白中加入被分析物標(biāo)樣Carriedthroughsamplepreparationprocess在樣品準(zhǔn)備過程中加入27FortifiedBlanks（增強空白）AnalyteSurrogate（替代）Compoundwithsimilarpropertiestotargetanalyte與被分析物具有相近特性的化合物Addedtoallsamples(unknownsandQC)butnotstandards在所有樣品(未知的和QC)中加入，但標(biāo)樣中不加Usedtomonitormethodperformanceonasample(matrix)specificbasis應(yīng)基于特定樣品（基體），用于監(jiān)測方法表現(xiàn)28Surrogate（替代）Compoundwithsim

ReferenceMaterials

參考物質(zhì)Matrixmatchedmaterialswithknownconcentrationofanalytes（被分析物已知濃度的基體匹配的物質(zhì)）Maybeexternalorin-house（外部或室內(nèi)）Sources（來源）NIST(US)NRC(Canada)EuropeanUnion（歐盟）CommercialVendors（商業(yè)渠道）29ReferenceMaterials

參考物質(zhì)MatriReferenceMaterials

參考物質(zhì)Usedprimarilytomonitoraccuracy主要用于監(jiān)測準(zhǔn)確度Maybeusedforotherquality用于其它質(zhì)量目的measures(precision,sensitivity)測量（精密度、靈敏度）BestoverallQC?（最好的全面質(zhì)量控制？）Expensive（費用高）30ReferenceMaterials

參考物質(zhì)UsedpPrecisionStudies（精密度研究）Duplicates（重復(fù)）Fieldduplicates（場地重復(fù)）Labduplicates（實驗室重復(fù)）Instrumentduplicates（儀器重復(fù)）Inter-labsplits（室內(nèi)分樣）Usedtoidentifyvarianceindifferentprocesses（用于識別不同過程的變異）31PrecisionStudies（精密度研究）DuplicSensitivityStudies

靈敏度研究Usuallyperformedinitially,thenperiodicallythereafter通常最開始要做，以后定期做Multiplereplicatesofablankorlow-levelstandard空白或低含量標(biāo)準(zhǔn)多次重復(fù)32SensitivityStudies

靈敏度研究UsualSensitivityStudies

靈敏度研究DetectionLimit–noquantitation檢測限-非定量QuantitationLimit–Accuracycriteriaadded定量限–準(zhǔn)確度準(zhǔn)則33SensitivityStudies

靈敏度研究DetecSensitivityStudies

靈敏度研究DetectionLimit–99%certaintythattheconcentrationisgreaterthanzero–thattheanalyteispresentinthesample（檢測限—99%確定濃度大于0-樣品中有被分析物）Uncertaintyishigh(+/-100%ormore)不確定度高（+/-100%或更高）QuantitationLimit（定量限）Lowestconcentrationthatcanbedeterminedwithagivenaccuracy(e.g.20%relativeerror)在一定準(zhǔn)確度下（如20%相對誤差）可以測定出的最低濃度34SensitivityStudies

靈敏度研究DetecLinearity（線性）Determinedinitiallyandthenasneeded最開始時測定，然后需要時測定DynamicLinearRangerelatestodetectorresponse動態(tài)線性范圍與檢測器響應(yīng)有關(guān)Alsoconsiderpreparationlimitations也可以認(rèn)為是準(zhǔn)備中的限制Solubilities（溶解度）Extractionefficiencies（提取率）Derivitizingreactions（衍生反應(yīng)）35Linearity（線性）DeterminedinitiaWhatdowerunasQC?

為什么要做質(zhì)量控制Itdependson:（取決于）Typeofinstrumentation儀器類型StageofMethodDevelopment方法開發(fā)階段Typeofanalysis分析類型36WhatdowerunasQC?

為什么要做質(zhì)量控WhatdowerunasQC?

為什么要做質(zhì)量控制StageofMethodDevelopment方法開發(fā)階段Validation（確認(rèn)）Verification/Qualification（驗證/判斷）Routineanalysis（日常分析）37WhatdowerunasQC?

為什么要做質(zhì)量控WhatdowerunasQC?

為什么要做質(zhì)量控制TypeofAnalysis（分析類型）Assay（分析）Impurities（雜質(zhì)）Limits（限制）Content（含量）Identification（識別）38WhatdowerunasQC?

為什么要做質(zhì)量控QualityDataRequiredatMethodValidation（方法確認(rèn)所需的質(zhì)量數(shù)據(jù)）

DataRequired所需數(shù)據(jù)I.D.名稱ImpurityTesting雜質(zhì)檢測AssayContent分析含量Quant.量Limit限Accuracy準(zhǔn)確度NOYESNOYESPrecision精密度NOYESNOYESSelectivity選擇性YESYESYESYESDetectionlimit檢測限NOMAYBE可能YESNOQuantitationlimit定量限NOYESNOMAYBE可能Linearity線性NOYESNOYESRange范圍NOYESNOYES39QualityDataRequiredatMethoQualityDataRequiredinRoutineAnalysis日常分析所需質(zhì)量數(shù)據(jù)DataRequired所需數(shù)據(jù)I.D.名稱ImpurityTesting雜質(zhì)檢測AssayContent分析含量Quant.量Limit限Accuracy準(zhǔn)確度NOYESNOYESPrecision精密度NOYESNOYESSelectivity選擇性NOMAYBE1NOMAYBE1Detectionlimit檢測限NONONONOQuantitationlimit定量限NOMAYBENOMAYBELinearity線性NOYESNOYESRange范圍NONONONO1–mayberequiredwhenworkinginunknownmatrix40QualityDataRequiredinRoutiReviewofQualityAssurance

質(zhì)量保證概述Wewillcover（內(nèi)容）DefinitionandDescriptionofQA質(zhì)量保證的定義和描述ToolsinaQASystem（QA體系的工具）ProficiencyTesting（能力驗證）CertifiedReferenceMaterials（有證標(biāo)準(zhǔn)物質(zhì)）ValidatedMethods（經(jīng)過確認(rèn)的方法）41ReviewofQualityAssurance

質(zhì)量

QualityAssurance（質(zhì)量保證）QualityAssurance質(zhì)量保證Plannedactionsdesignedtoprovideconfidencethatqualityrequirementswillbefulfilled為質(zhì)量要求得到滿足提供信心而設(shè)計的有計劃的活動QualityAssuranceSystem質(zhì)量保證體系A(chǔ)setofprocessesappliedwithinadefinedstructuretogeneratedesiredoutcomes在規(guī)定的結(jié)構(gòu)內(nèi)產(chǎn)生預(yù)期結(jié)果所采用的一組過程Thegoodmanagementofgoodscience良好的科學(xué)良好的管理42QualityAssurance（質(zhì)量保證）QualitQualitySystemComponents

質(zhì)量體系組成Management管理Plan策劃Performance實施Do做Assessment評價Review評審43QualitySystemComponents

質(zhì)量體系6PillarsofQA/QC

QA/QC的六個基礎(chǔ)Management管理Facilities設(shè)施Personnel人員CRM’s有證標(biāo)準(zhǔn)物質(zhì)PT’s能力驗證ValidatedMethods經(jīng)確認(rèn)的方法446PillarsofQA/QC

QA/QC的六個基礎(chǔ)MProficiencyTesting能力驗證Providesexternalassessmentofperformance為表現(xiàn)提供外部評審Providesabasisforcorrectiveandpreventiveaction為糾正和預(yù)防措施提供基礎(chǔ)45ProficiencyTesting能力驗證ProvideInformationGained

搜集信息Comparisonofperformanceagainstanexternalstandard將表現(xiàn)與外部標(biāo)準(zhǔn)比較Comparisonagainstpastperformance與過去的表現(xiàn)比較Comparisonagainstpeer(competitor)labs與同行（競爭者比較）Identificationofunsatisfactoryperformers識別出不滿意的操作者46InformationGained

搜集信息CompariTypesofPT

能力驗證類型Specificanalyte/matrixcombination特定被分析物/基體結(jié)合Mercuryinfish（魚中的汞）Benzeneinair（空氣中的苯）Fieldofanalysis（場地分析）MetalsbyICP（ICP測金屬）PesticidesbyGC/MS（GC/MS測殺蟲劑）47TypesofPT

能力驗證類型SpecificanaSamples樣品Sub-sampledfrombulksupply從批中抽取樣本Discretesamplesplitanddistributed謹(jǐn)慎分割樣品并分發(fā)48Samples樣品Sub-sampledfrombulkInterlaboratoryComparisons

實驗室間比對Collaborativestudies協(xié)同研究Certificationstudies認(rèn)證研究Round-robinstudies循環(huán)研究49InterlaboratoryComparisons

實驗SelectionofPTprograms

PT方案的選擇Availabilityofrelevantprograms是否有相關(guān)方案Organizationofrelevantprograms相關(guān)方案的組織Anyprogramisusuallybetterthannothing只有要方案，總比沒有好50SelectionofPTprograms

PT方案的AssessmentofPTPrograms

PT方案的評價Beforecommittinglong-termconsider在實施前應(yīng)考慮Statisticsusedtointerpretdata解釋結(jié)果的統(tǒng)計技術(shù)How“true”valueisdetermined真值如何確定Theoretical理論值Refereelab參考實驗室Consensus公議值51AssessmentofPTPrograms

PT方案ScoringofParticipants

參加者的評價Z–score（Z值）Deviationfrom“true”valuedividedbysigma測得值與真值之差除以σSigmamaybeanaccepteddeviationorstatisticallydeterminedineachroundσ可能是可接受的偏差或每輪測試的統(tǒng)計結(jié)果52ScoringofParticipants

參加者的評價Scoring

Z-值GenerallyaZ-score（Z-值）<2isconsideredsatisfactory（滿意）>2,<3isconsideredquestionable（可疑）>3isconsideredunsatisfactory（離群）scoresmustbewithin2–sigmaZ-值必須在2-σ之間53Scoring

Z-值GenerallyaZ-scoreLaboratoryInterpretation

實驗室的解釋Viewresultsincontext（從整體上看結(jié)果）Dotheyagreewithin-houseQCdata是否與室內(nèi)質(zhì)量控制數(shù)據(jù)一致Trendanalysis(considerhowsigmaisdetermined)趨勢分析（考慮σ是如何確定的）Performanceofotherparticipants其它參加者的表現(xiàn)54LaboratoryInterpretation

實驗室的LaboratoryInterpretation

實驗室的解釋Comparemethodologyandre-calculateifpossible比較方法，如果可能重新計算Compareuncertaintyagainstin-houseestimates將不確定度與室內(nèi)評估比較55LaboratoryInterpretation

實驗室的CorrectiveActions

糾正措施Determinewhentotakeaction確定何時采取措施After1unsatisfactoryscore?一個不滿意結(jié)果Aftermany(3)inoneround?一輪中多個（如三個）不滿意結(jié)果After2consecutiveunsatisfactoryscores?連續(xù)二個不滿意結(jié)果56CorrectiveActions

糾正措施DetermiCorrectiveActions

糾正措施Alwaysinvestigate總要調(diào)查Include包括QCdata質(zhì)量控制數(shù)據(jù)Calculations,dilutions,transcriptions計算、稀釋，抄寫Trainingstatusofanalyst分析人員培訓(xùn)狀況Performancerecordsofequipment設(shè)備運行記錄Recordsofcalibrants,reagentsetc.校準(zhǔn)品、試劑的記錄等57CorrectiveActions

糾正措施AlwaysCorrectiveActions

糾正措施Formulateaction公布措施Executeaction實施措施Checkifactionwassuccessful檢查措施是否有效58CorrectiveActions

糾正措施FormulaGeneralConsiderations

幾點考慮MoreemphasisisbeingplacedonPTprogramsbyassessors,regulatorsandclients評審員、管理部門和客戶更多強調(diào)PTUsealltheinformationavailable利用所有可得到的信息HandlePT’slikeroutinesamples(asmuchaspossible)象常規(guī)樣品一樣處理PT樣品（盡可能）59GeneralConsiderations

幾點考慮MorThirdPartyAssessment

第三方評審AccreditationBodies認(rèn)可機構(gòu)AssessperformanceagainstlaboratoryscoperatherthanPTprogramcriteria在一定范圍內(nèi)評審實驗室的表現(xiàn)，而不是PT方案準(zhǔn)則Consider“fitforpurpose”考慮適宜性60ThirdPartyAssessment

第三方評審AcThirdPartyAssessment

第三方評審Regulators政府管理部門MaybeinvolvedindevelopmentofPTprograms可能參與PT方案的開發(fā)Mayrequireassistancefromprogramcoordinatortoassessresults可能需要方案協(xié)調(diào)人來幫助評審結(jié)果61ThirdPartyAssessment

第三方評審ReThirdPartyAssessment

第三方評審Customers客戶WhenusingPTresultsasaperformancestandardensuretargetisrealistic當(dāng)使用PT結(jié)果作為能力標(biāo)準(zhǔn)時，確保目標(biāo)是現(xiàn)實的Mustinvestigateprogram;notjustresults必須調(diào)查方案，而不僅是結(jié)果62ThirdPartyAssessment

第三方評審CuReferenceMaterials

參考物質(zhì)5types（5種類型）Puresubstance（純物質(zhì)）Standardsolutionsandgasmixtures（標(biāo)準(zhǔn)溶液和氣體混合物）MatrixRM’s（基體參考物質(zhì)）Physicalproperties（物理特性）Referenceobjects(artifacts)（參考目標(biāo)）（參考品）63ReferenceMaterials

參考物質(zhì)5typeReferenceMaterials

參考物質(zhì)Maybeusedfor可用于InternalQC內(nèi)部質(zhì)量控制Methodvalidation方法確認(rèn)Calibration校準(zhǔn)Estimatinguncertainty評估不確定度Training培訓(xùn)64ReferenceMaterials

參考物質(zhì)MaybeClassification分類CertifiedReferenceMaterials有證參考物質(zhì)Directlytraceable直接溯源Eachpropertyhasanuncertaintyassociatedwithit每一特性有相應(yīng)不確定度Referencematerial參考物質(zhì)Propertiesarehomogenousandthoroughlycharacterizedtobeusedforcalibrationormethodassessment特性是均勻的，并完整定值，以用于校準(zhǔn)或方法評價65Classification分類CertifiedRefeAvailability可獲得性Generallypoorthereforeexpensive(不容易獲得,費用高)Governmentagencies政府機構(gòu)NIST,NRC,EU-BCRTradeassociations貿(mào)易協(xié)會AOAC,AOCA(OilChemists)石油化學(xué)Commercialsuppliers商業(yè)供貨商66Availability可獲得性GenerallypoorRMinValidation

方法確認(rèn)中參考物質(zhì)的使用Estimationofbiasbetweenmethodandtruevalue評估方法和真值間的偏差Estimationofbiasbetweentwomethods評估方法間的偏差RequireslessrigorouslycertifiedRM要求的有證標(biāo)準(zhǔn)物質(zhì)相對不是太嚴(yán)格Limitedbyuncertaintyofcertifiedvalues受參考值不確定度的限制67RMinValidation

方法確認(rèn)中參考物質(zhì)的使用ERMinValidation

參考物質(zhì)在方法確認(rèn)中的應(yīng)用MatrixRMmustbewithinscopeofthemethod參考物質(zhì)的基體必須適用于該方法MultipleRM’smayberequiredtocoverrangeofmethod含多種成分的參考物質(zhì)應(yīng)適用于該方法68RMinValidation

參考物質(zhì)在方法確認(rèn)中的應(yīng)用RMinCalibration

參考物質(zhì)在方法校正中的應(yīng)用Usuallyusepuresubstance常用純物質(zhì)Uncertaintyassociatedwithpuritywillcontributetouncertaintyofthemethod與純度相關(guān)的不確定度是方法不確定度的分量SomemethodologyrequiresRMforcalibrationofentireprocess(XRF)有些方法學(xué)需要用參考物質(zhì)對整個過程校準(zhǔn)(XRF)69RMinCalibration

參考物質(zhì)在方法校正中的應(yīng)RMinTraining

參考物質(zhì)在方法培訓(xùn)中的應(yīng)用Qualifyingnewanalysts培養(yǎng)合格的新分析人員Checkingmethodsusedinfrequently檢查不常用的分析方法Troubleshootingmethods解決分析方法中的疑難問題70RMinTraining

參考物質(zhì)在方法培訓(xùn)中的應(yīng)用QuRMasQC

參考物質(zhì)用于質(zhì)量控制Mustbecharacterizedwithrespecttostabilityandhomogeneity必須穩(wěn)定、均勻,認(rèn)定特征值71RMasQC

參考物質(zhì)用于質(zhì)量控制MustbechaSuitability適用性Matrixmatch(interferences)基體匹配程度(干擾)Concentrationrange濃度范圍Uncertaintyofcertifiedvalues參考值的不確定度Source(conformancewithstandards)來源(與標(biāo)準(zhǔn)的符合性)Ongoingavailability目前是否可得到But–Howtoassess但是–如何進行評估呢?72Suitability適用性Matrixmatch(inIn-houseproduction

內(nèi)部研究Whatwouldtherequirementsbe需要具備哪些必要條件?73In-houseproduction

內(nèi)部研究Whatw

ReviewofQualityControl

質(zhì)量控制概要Wewillcover(內(nèi)容)Terminology術(shù)語CharacteristicsofAnalyticalMethods分析方法特性TypesofQCsamplesandhowtheyrelatetothecharacteristicsQC樣品類型和特性74ReviewofQualityControl

質(zhì)量控DefinitionofQuality

質(zhì)量的定義Tomostoftheworld(普遍上)degreeofexcellence(優(yōu)異程度)TotheISOworld(在ISO領(lǐng)域)degreeofagreementbetweencharacteristicsandrequirements特性與要求的吻合程度Moreimportantly(更重要)toourclients?(對客戶)75DefinitionofQuality

質(zhì)量的定義ToQualityControlvs.QualityAssurance(質(zhì)量控制與質(zhì)量保證)Qualitycontrolisaseriesofmeasurementsusedtoassessthequalityoftheanalyticaldata質(zhì)量控制是一系列測量,以評價分析數(shù)據(jù)的質(zhì)量Howwellisthetestfulfilling

requirements?試驗滿足要求的程度如何?76QualityControlvs.QualityAsQualityControlvs.QualityAssurance(質(zhì)量控制與質(zhì)量保證)Qualityassuranceisamanagementplantoensuretheintegrityofdata(asystem)質(zhì)量保證是一種管理計劃,以確保數(shù)據(jù)的完整性(一種體系)Providesconfidencethatrequirementswillbefulfilled為要求是否得到滿足提供信心77QualityControlvs.QualityAsQualitiesofAnalyticalMethods

分析方法的質(zhì)量Accuracy(準(zhǔn)確度)Precision(精密度)Selectivity(選擇性)Sensitivity(靈敏度)Linearity(線性)Range(范圍)Robustness/Ruggedness(穩(wěn)健性/穩(wěn)度)78QualitiesofAnalyticalMethoAccuracy(準(zhǔn)確度)Degreeofagreementbetweenthe“true”valueandthemeasuredvalue(真值與測量值之間的一致程度)79Accuracy(準(zhǔn)確度)DegreeofagreemeAccuracy(準(zhǔn)確度)Whatisthe“true”value?(什么是真值)Theoretical(理論值)Consensus(公議值)Accepted/Assigned(可接受/賦值)80Accuracy(準(zhǔn)確度)7Accuracy(準(zhǔn)確度)Expressedas(表示為)theratiobetweentheassayedvalueandthe“true”value(%recovery)分析值與真值間的比(%回收率)thedifferencebetweentheassayandtheacceptedtruevalue(%Error)分析與可接受真值間的差(%誤差)81Accuracy(準(zhǔn)確度)Expressedas(表示Precision(精密度)Closenessofagreementbetweenmeasurements(測量間的一致程度)Repeatability(r)–sameconditions,shorttimeinterval(samerun)–shorttermprecision重復(fù)性(r)-相同條件下\短時間間隔-短期內(nèi)精密度Intermediateprecision–samelabdifferentday,analyst,instrument中間精密度-同一實驗室不同日期,分析人員,儀器Reproducibility(R)–agreementbetweenbatchesorbetweenlabs復(fù)現(xiàn)性?-批間或?qū)嶒炇议g的一致性82Precision(精密度)ClosenessofagrPrecision(精密度)ExpressedasStandardDeviation,RelativeStandardDeviationorRelativePercentDifference表示為標(biāo)準(zhǔn)偏差、相對標(biāo)準(zhǔn)偏差、相對百分差83Precision(精密度)ExpressedasStSensitivity（靈敏度）Degreeofresponsetoachangeinanalyteconcentration–resolution被分析物濃度變化的響應(yīng)變化程度-分辯率Lowestconcentrationthatcanbedistinguishedfrombackgroundnoise–detectionlimit能從背景噪音識別出的最低濃度-檢測限84Sensitivity（靈敏度）DegreeofrespSensitivity（靈敏度）Limitofdetectionvs.Limitofquantification（檢測限與定量限）Limitofdetection(LOD)isthelevelthatwecansaywhetherananalyteispresentornot檢測限是我們判斷被分析物是否存在的含量水平Limitofquantitation(LOQ)isthelevelthatwecanquantifytheanalytewithaspecifiedaccuracy(20%)定量限是我們按規(guī)定準(zhǔn)確度（20%）能對被分析物量化的含量水平85Sensitivity（靈敏度）LimitofdeteSelectivity（選擇性）Abilitytodetecttheanalyteinacomplexmatrix檢測復(fù)雜基體中被析物的能力Abilitytoexcludenon-analytespeciesfromsignal通過信號排除非被分析物的能力Usuallyinverselyrelatedtosensitivity通常與靈敏度成反比86Selectivity（選擇性）AbilitytodetLinearity（線性）Abilitytoproducearesponsethatisdirectlyproportionaltotheconcentrationoftheanalyte所產(chǎn)生的反應(yīng)與被分析物濃度成正比的能力Onlyholdstruewithinagivenrange只在給定范圍內(nèi)是真實的87Linearity（線性）AbilitytoproducLinearity（線性）Expressedascorrelationcoefficient(r)orcoefficientofdetermination(r2)表示為相關(guān)系數(shù)(r)或測定系數(shù)(r2)r2=ssxy2/ssxxssyy88Linearity（線性）ExpressedascorRange（范圍）Theintervalbetweenthehighestandlowestconcentrationforwhichthemethodhasshowntohavesuitablelevelsofaccuracy,precisionandlinearity.在方法具有適宜的準(zhǔn)確度、精密度和線性的條件下，最高和最低濃度范圍89Range（范圍）TheintervalbetweenRobustness（穩(wěn)健性）Abilityofmethodtobeunaffectedbysmallchangesinmethod(internal)conditions（方法不因條件的較小變化（內(nèi)部）而受影響的能力）Temperature（溫度）pHCompositionofmobilephase（流動相組成）Usefulwhenmethodmovesfromdevelopmenttoproduction（從方法開發(fā)到使用很有用）90Robustness（穩(wěn)健性）AbilityofmethRuggedness（穩(wěn)度）Abilityofmethodtobeunaffectedbyexternalconditions（方法不受外界條件影響的能力）Differentanalysts（不同的分析人員）Differentlaboratories（不同的實驗室）Differentreagentlots（不同批的試劑）Differentinstruments（不同的儀器）91Ruggedness（穩(wěn)度）AbilityofmethoRuggedness（穩(wěn)度）Usefulfortechnologytransfer（對技術(shù)推廣很有用）92Ruggedness（穩(wěn)度）UsefulfortechQualityControlMeasures

質(zhì)量控制手段Calibrationstandards（校準(zhǔn)標(biāo)準(zhǔn)）Blanks（空白）Recoverystudies（回收率研究）Precisionstudies（精密度研究）Sensitivitystudies（靈敏度研究）DetectionLimit（檢測限）Quantitationlimit（定量限）93QualityControlMeasures

質(zhì)量控制手

Calibration(校準(zhǔn))Directlyaffectsaccuracy(直接影響準(zhǔn)確度)Preparationofstandards(標(biāo)準(zhǔn)制備)Matrix(基體)Stability(穩(wěn)定性)Signaltype:peakarea,peakheight信號類型:峰面積,峰高94Calibration(校準(zhǔn))DirectlyaffeCalibration(校準(zhǔn))Calibrationcurves(校準(zhǔn)曲線)1storder–straightline(一級-直線)Quadratic–acceptablebutrequiresmorepoints(二次方程-可以接受,但需要更多點)Internalstandards(內(nèi)標(biāo))Refinescalibrationresponse(增強校準(zhǔn)響應(yīng))Addedtosamplesandstandards(加入樣品和標(biāo)準(zhǔn)中)Mustbehaveliketheanalyte(象被分析物一樣表現(xiàn))Cannotbeinsamples–rareelements,deuteratedcompounds(樣品中沒有-稀有元素,含重氘的化合物)95Calibration(校準(zhǔn))CalibrationcuCalibration(校準(zhǔn))Calibrationverification(校準(zhǔn)驗證)Repeatedcalibrationstandard重復(fù)校準(zhǔn)標(biāo)準(zhǔn)Intervalmaybeevery20samples(ICPMS)oronceeveryrun(GC-FID)間隔:20個樣品(ICPMS)每次(GC-FID)96Calibration(校準(zhǔn))CalibrationveBlanks(空白)Usedtomonitorcontamination(監(jiān)測污染)Reagentblanks(試劑空白)Instrumentblanks(儀器空白)Fieldblanks(場地空白)Tripblanks(路途空白)Procedural/methodblanks(程序/方法空白)Matrixblanks(基體空白)Others?(其它)97Blanks(空白)UsedtomonitorcontRecoveryStudies（回收率研究）Usedtomonitoraccuracy（監(jiān)測準(zhǔn)確度）Matrixspikes（基體加標(biāo)）Fortifiedblanks（增加加標(biāo)）Surrogates（替代）ReferenceMaterials（參考物質(zhì)）98RecoveryStudies（回收率研究）UsedtoMatrixSpikes（基體加標(biāo)）Knownamountofanalyteaddedtosample在樣品中加入已知量的被分析物Importantwithcomplexmatrix對復(fù)雜基體很重要Generallyaddedpriortoextractionprocess（通常在提取前加入）Sometimesdifficulttoknowamounttospikeaheadoftime（有時很難提前知道加標(biāo)量）99MatrixSpikes（基體加標(biāo)）KnownamounFortifiedBlanks（增強空白）Analytespikeintoreagentblank在試劑空白中加入被分析物標(biāo)樣Carriedthroughsamplepreparationprocess在樣品準(zhǔn)備過程中加入100FortifiedBlanks（增強空白）AnalyteSurrogate（替代）Compoundwithsimilarpropertiestotargetanalyte與被分析物具有相近特性的化合物Addedtoallsamples(unknownsandQC)butnotstandards在所有樣品(未知的和QC)中加入，但標(biāo)樣中不加Usedtomonitormethodperformanceonasample(matrix)specificbasis應(yīng)基于特定樣品（基體），用于監(jiān)測方法表現(xiàn)101Surrogate（替代）Compoundwithsim

ReferenceMaterials

參考物質(zhì)Matrixmatchedmaterialswithknownconcentrationofanalytes（被分析物已知濃度的基體匹配的物質(zhì)）Maybeexternalorin-house（外部或室內(nèi)）Sources（來源）NIST(US)NRC(Canada)EuropeanUnion（歐盟）CommercialVendors（商業(yè)渠道）102ReferenceMaterials

參考物質(zhì)MatriReferenceMaterials

參考物質(zhì)Usedprimarilytomonitoraccuracy主要用于監(jiān)測準(zhǔn)確度Maybeusedforotherquality用于其它質(zhì)量目的measures(precision,sensitivity)測量（精密度、靈敏度）BestoverallQC?（最好的全面質(zhì)量控制？）Expensive（費用高）103ReferenceMaterials

參考物質(zhì)UsedpPrecisionStudies（精密度研究）Duplicates（重復(fù)）Fieldduplicates（場地重復(fù)）Labduplicates（實驗室重復(fù)）Instrumentduplicates（儀器重復(fù)）Inter-labsplits（室內(nèi)分樣）Usedtoidentifyvarianceindifferentprocesses（用于識別不同過程的變異）104PrecisionStudies（精密度研究）DuplicSensitivityStudies

靈敏度研究Usuallyperformedinitially,thenperiodicallythereafter通常最開始要做，以后定期做Multiplereplicatesofablankorlow-levelstandard空白或低含量標(biāo)準(zhǔn)多次重復(fù)105SensitivityStudies

靈敏度研究UsualSensitivityStudies

靈敏度研究DetectionLimit–noquantitation檢測限-非定量QuantitationLimit–Accuracycriteriaadded定量限–準(zhǔn)確度準(zhǔn)則106SensitivityStudies

靈敏度研究DetecSensitivityStudies

靈敏度研究DetectionLimit–99%certaintythattheconcentrationisgreaterthanzero–thattheanalyteispresentinthesample（檢測限—99%確定濃度大于0-樣品中有被分析物）Uncertaintyishigh(+/-100%ormore)不確定度高（+/-100%或更高）QuantitationLimit（定量限）Lowestconcentrationthatcanbedeterminedwithagivenaccuracy(e.g.20%relativeerror)在一定準(zhǔn)確度下（如20%相對誤差）可以測定出的最低濃度107SensitivityStudies

靈敏度研究DetecLinearity（線性）Determinedinitiallyandthenasneeded最開始時測定，然后需要時測定DynamicLinearRangerelatestodetectorresponse動態(tài)線性范圍與檢測器響應(yīng)有關(guān)Alsoconsiderpreparationlimitations也可以認(rèn)為是準(zhǔn)備中的限制Solubilities（溶解度）Extractionefficiencies（提取率）Derivitizingreactions（衍生反應(yīng)）108Linearity（線性）DeterminedinitiaWhatdowerunasQC?

為什么要做質(zhì)量控制Itdependson:（取決于）Typeofinstrumentation儀器類型StageofMethodDevelopment方法開發(fā)階段Typeofanalysis分析類型109WhatdowerunasQC?

為什么要做質(zhì)量控WhatdowerunasQC?

為什么要做質(zhì)量控制StageofMethodDevelopment方法開發(fā)階段Validation（確認(rèn)）Verification/Qualification（驗證/判斷）Routineanalysis（日常分析）110WhatdowerunasQC?

為什么要做質(zhì)量控WhatdowerunasQC?

為什么要做質(zhì)量控制TypeofAnalysis（分析類型）Assay（分析）Impurities（雜質(zhì)）Limits（限制）Content（含量）Identification（識別）111WhatdowerunasQC?

為什么要做質(zhì)量控QualityDataRequiredatMethodValidation（方法確認(rèn)所需的質(zhì)量數(shù)據(jù)）

DataRequired所需數(shù)據(jù)I.D.名稱ImpurityTesting雜質(zhì)檢測AssayContent分析含量Quant.量Limit限Accuracy準(zhǔn)確度NOYESNOYESPrecision精密度NOYESNOYESSelectivity選擇性YESYESYESYESDetectionlimit檢測限NOMAYBE可能YESNOQuantitationlimit定量限NOYESNOMAYBE可能Linearity線性NOYESNOYESRange范圍NOYESNOYES112QualityDataRequiredatMethoQualityDataRequiredinRoutineAnalysis日常分析所需質(zhì)量數(shù)據(jù)DataRequired所需數(shù)據(jù)I.D.名稱ImpurityTesting雜質(zhì)檢測AssayContent分析含量Quant.量Limit限Accuracy準(zhǔn)確度NOYESNOYESPrecision精密度NOYESNOYESSelectivity選擇性NOMAYBE1NOMAYBE1Detectionlimit檢測限NONONONOQuantitationlimit定量限NOMAYBENOMAYBELinearity線性NOYESNOYESRange范圍NONONONO1–mayberequiredwhenworkinginunknownmatrix113QualityDataRequiredinRoutiReviewofQualityAssurance

質(zhì)量保證概述Wewillcover（內(nèi)容）DefinitionandDescriptionofQA質(zhì)量保證的定義和描述ToolsinaQASystem（QA體系的工具