質(zhì)量控制概要中英文

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1DefinitionofQuality

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(duì)客戶)2QualityControlvs.QualityAssurance(質(zhì)量控制與質(zhì)量保證)Qualitycontrolisaseriesofmeasurementsusedtoassessthequalityoftheanalyticaldata質(zhì)量控制是一系列測(cè)量,以評(píng)價(jià)分析數(shù)據(jù)的質(zhì)量Howwellisthetestfulfilling

requirements?試驗(yàn)滿足要求的程度如何?3QualityControlvs.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(jì)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4QualitiesofAnalyticalMethods

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)5Accuracy(準(zhǔn)確度)Degreeofagreementbetweenthe“true”valueandthemeasuredvalue(真值與測(cè)量值之間的一致程度)6Accuracy(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)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)8Precision(精密度)Closenessofagreementbetweenmeasurements(測(cè)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(shí)間間隔-短期內(nèi)精密度Intermediateprecision–samelabdifferentday,analyst,instrument中間精密度-同一實(shí)驗(yàn)室不同日期,分析人員,儀器Reproducibility(R)–agreementbetweenbatchesorbetweenlabs復(fù)現(xiàn)性?-批間或?qū)嶒?yàn)室間的一致性9Precision(精密度)ExpressedasStandardDeviation,RelativeStandardDeviationorRelativePercentDifference表示為標(biāo)準(zhǔn)偏差、相對(duì)標(biāo)準(zhǔn)偏差、相對(duì)百分差10Sensitivity（靈敏度度）Degreeofresponsetoachangeinanalyteconcentration––resolution被分析析物濃濃度變變化的的響應(yīng)應(yīng)變化化程度度-分分辯率率Lowestconcentrationthatcanbedistinguishedfrombackgroundnoise––detectionlimit能從背背景噪噪音識(shí)識(shí)別出出的最最低濃濃度-檢測(cè)測(cè)限11Sensitivity（（靈敏度度）Limitofdetectionvs.Limitofquantification（（檢測(cè)限限與定定量限限）Limitofdetection(LOD)isthelevelthatwecansaywhetherananalyteispresentornot檢測(cè)限限是我我們判判斷被被分析析物是是否存存在的的含量量水平平Limitofquantitation(LOQ)isthelevelthatwecanquantifytheanalytewithaspecifiedaccuracy(20%)定量限是我我們按規(guī)定定準(zhǔn)確度（（20%））能對(duì)被分分析物量化化的含量水水平12Selectivity（選擇性）Abilitytodetecttheanalyteinacomplexmatrix檢測(cè)復(fù)雜基基體中被析析物的能力力Abilitytoexcludenon-analytespeciesfromsignal通過信號(hào)排排除非被分分析物的能能力Usuallyinverselyrelatedtosensitivity通常與靈敏敏度成反比比13Linearity（線性）Abilitytoproducearesponsethatisdirectlyproportionaltotheconcentrationoftheanalyte所產(chǎn)生的反反應(yīng)與被分分析物濃度度成正比的的能力Onlyholdstruewithinagivenrange只在給定范范圍內(nèi)是真真實(shí)的14Linearity（線性）Expressedascorrelationcoefficient(r)orcoefficientofdetermination(r2)表示為相相關(guān)系數(shù)數(shù)(r)或測(cè)定系系數(shù)(r2)r2=ssxy2/ssxxssyy15Range（范圍）Theintervalbetweenthehighestandlowestconcentrationforwhichthemethodhasshowntohavesuitablelevelsofaccuracy,precisionandlinearity.在方法具具有適宜宜的準(zhǔn)確確度、精精密度和和線性的的條件下下，最高高和最低低濃度范范圍16Robustness（穩(wěn)健性））Abilityofmethodtobeunaffectedbysmallchangesinmethod(internal)conditions（方法不因因條件的的較小變變化（內(nèi)內(nèi)部）而而受影響響的能力力）Temperature（溫度）pHCompositionofmobilephase（（流動(dòng)相組組成）Usefulwhenmethodmovesfromdevelopmenttoproduction（從方法開開發(fā)到使使用很有有用）17Ruggedness（穩(wěn)度）Abilityofmethodtobeunaffectedbyexternalconditions（（方法不受受外界條條件影響響的能力力）Differentanalysts（（不同的分分析人員員）Differentlaboratories（不同的實(shí)實(shí)驗(yàn)室））Differentreagentlots（不同批的的試劑））Differentinstruments（（不同的儀儀器）18Ruggedness（穩(wěn)度）Usefulfortechnologytransfer（（對(duì)技術(shù)推推廣很有有用）19QualityControlMeasures質(zhì)量控制制手段Calibrationstandards（（校準(zhǔn)標(biāo)準(zhǔn)準(zhǔn)）Blanks（（空白）Recoverystudies（回收率研研究）Precisionstudies（精密度研研究）Sensitivitystudies（靈敏度研研究）DetectionLimit（（檢測(cè)限））Quantitationlimit（（定量限））20Calibration(校準(zhǔn))Directlyaffectsaccuracy(直接影響響準(zhǔn)確度度)Preparationofstandards(標(biāo)準(zhǔn)制備備)Matrix(基體)Stability(穩(wěn)定性)Signaltype:peakarea,peakheight信號(hào)類型型:峰面面積,峰峰高21Calibration(校準(zhǔn))Calibrationcurves(校準(zhǔn)曲線線)1storder––straightline(一級(jí)-直直線)Quadratic––acceptablebutrequiresmorepoints(二次方程程-可以以接受,但需要要更多點(diǎn)點(diǎn))Internalstandards(內(nèi)標(biāo))Refinescalibrationresponse(增強(qiáng)校準(zhǔn)準(zhǔn)響應(yīng))Addedtosamplesandstandards(加入樣品品和標(biāo)準(zhǔn)準(zhǔn)中)Mustbehaveliketheanalyte(象被分析析物一樣樣表現(xiàn))Cannotbeinsamples––rareelements,deuteratedcompounds(樣品中沒沒有-稀稀有元素素,含重重氘的化化合物)22Calibration(校準(zhǔn))Calibrationverification(校準(zhǔn)驗(yàn)證證)Repeatedcalibrationstandard重復(fù)校準(zhǔn)標(biāo)標(biāo)準(zhǔn)Intervalmaybeevery20samples(ICPMS)oronceeveryrun(GC-FID)間隔:20個(gè)樣品(ICPMS)每次(GC-FID)23Blanks(空白)Usedtomonitorcontamination(監(jiān)測(cè)污染)Reagentblanks(試劑空白)Instrumentblanks(儀器空白)Fieldblanks(場(chǎng)地空白)Tripblanks(路途空白)Procedural/methodblanks(程序/方法法空白)Matrixblanks(基體空白)Others?(其它)24RecoveryStudies（（回收率研究究）Usedtomonitoraccuracy（（監(jiān)測(cè)準(zhǔn)確度度）Matrixspikes（（基體體加加標(biāo)標(biāo)））Fortifiedblanks（（增加加加加標(biāo)標(biāo)））Surrogates（（替代代））ReferenceMaterials（（參考考物物質(zhì)質(zhì)））25MatrixSpikes（（基體體加加標(biāo)標(biāo)））Knownamountofanalyteaddedtosample在樣樣品品中中加加入入已已知知量量的的被被分分析析物物Importantwithcomplexmatrix對(duì)復(fù)復(fù)雜雜基基體體很很重重要要Generallyaddedpriortoextractionprocess（通常在提取前前加入）Sometimesdifficulttoknowamounttospikeaheadoftime（有時(shí)很難提前前知道加標(biāo)量量）26FortifiedBlanks（增強(qiáng)空白）Analytespikeintoreagentblank在試劑空白中中加入被分析析物標(biāo)樣Carriedthroughsamplepreparationprocess在樣品準(zhǔn)備過過程中加入27Surrogate（替代）Compoundwithsimilarpropertiestotargetanalyte與被分析物具具有相近特性性的化合物Addedtoallsamples(unknownsandQC)butnotstandards在所有樣品(未知的和QC)中加入，但標(biāo)標(biāo)樣中不加Usedtomonitormethodperformanceonasample(matrix)specificbasis應(yīng)基于特定樣樣品（基體）），用于監(jiān)測(cè)測(cè)方法表現(xiàn)28ReferenceMaterials參考物質(zhì)Matrixmatchedmaterialswithknownconcentrationofanalytes（被分析物已知知濃度的基體體匹配的物質(zhì)質(zhì)）Maybeexternalorin-house（外部或或室室內(nèi)））Sources（來源））NIST(US)NRC(Canada)EuropeanUnion（（歐盟））CommercialVendors（（商業(yè)渠渠道））29ReferenceMaterials參考物物質(zhì)Usedprimarilytomonitoraccuracy主要用用于監(jiān)監(jiān)測(cè)準(zhǔn)準(zhǔn)確度度Maybeusedforotherquality用于其其它質(zhì)質(zhì)量目目的measures(precision,sensitivity)測(cè)量（（精密密度、、靈敏敏度））BestoverallQC?（（最好的的全面面質(zhì)量量控制制？））Expensive（費(fèi)用高高）30PrecisionStudies（精密度度研究究）Duplicates（（重復(fù)））Fieldduplicates（（場(chǎng)地重重復(fù)））Labduplicates（（實(shí)驗(yàn)室室重復(fù)復(fù)）Instrumentduplicates（儀器重重復(fù)））Inter-labsplits（（室內(nèi)分分樣））Usedtoidentifyvarianceindifferentprocesses（（用于識(shí)識(shí)別不不同過過程的的變異異）31SensitivityStudies靈敏度度研究究Usuallyperformedinitially,thenperiodicallythereafter通常最最開始始要做做，以以后定定期做做Multiplereplicatesofablankorlow-levelstandard空白或或低含含量標(biāo)標(biāo)準(zhǔn)多多次重重復(fù)32SensitivityStudies靈敏度度研究究DetectionLimit––noquantitation檢測(cè)限限-非非定量量QuantitationLimit––Accuracycriteriaadded定量限限–準(zhǔn)確度度準(zhǔn)則則33SensitivityStudies靈敏度度研究究DetectionLimit––99%certaintythattheconcentrationisgreaterthanzero––thattheanalyteispresentinthesample（檢測(cè)限限—99%確定定濃度度大于于0-樣品品中有有被分分析物物）Uncertaintyishigh(+/-100%ormore)不確定定度高高（+/-100%或更高高）QuantitationLimit（（定量限限）Lowestconcentrationthatcanbedeterminedwithagivenaccuracy(e.g.20%relativeerror)在一定定準(zhǔn)確確度下下（如如20%相相對(duì)誤誤差））可以以測(cè)定定出的的最低低濃度度34Linearity（線性））Determinedinitiallyandthenasneeded最開始始時(shí)測(cè)測(cè)定，，然后后需要要時(shí)測(cè)測(cè)定DynamicLinearRangerelatestodetectorresponse動(dòng)態(tài)線線性范范圍與與檢測(cè)測(cè)器響響應(yīng)有有關(guān)Alsoconsiderpreparationlimitations也可可以以認(rèn)認(rèn)為為是是準(zhǔn)準(zhǔn)備備中中的的限限制制Solubilities（（溶解度））Extractionefficiencies（提取率））Derivitizingreactions（衍生反應(yīng)應(yīng)）35WhatdowerunasQC?為什么要要做質(zhì)量量控制Itdependson:（取決于））Typeofinstrumentation儀器類型型StageofMethodDevelopment方法開發(fā)發(fā)階段Typeofanalysis分析類型型36WhatdowerunasQC?為什么要要做質(zhì)量量控制StageofMethodDevelopment方法開發(fā)發(fā)階段Validation（確認(rèn)）Verification/Qualification（驗(yàn)證/判判斷）Routineanalysis（日常分析析）37WhatdowerunasQC?為什么要要做質(zhì)量量控制TypeofAnalysis（分析類型型）Assay（分析）Impurities（雜質(zhì)）Limits（（限制）Content（含量）Identification（識(shí)別）38QualityDataRequiredatMethodValidation（（方法確認(rèn)認(rèn)所需的的質(zhì)量數(shù)數(shù)據(jù)）DataRequired所需數(shù)據(jù)I.D.名稱ImpurityTesting雜質(zhì)檢測(cè)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(cè)限NOMAYBE可能YESNOQuantitationlimit定量限NOYESNOMAYBE可能Linearity線性NOYESNOYESRange范圍NOYESNOYES39QualityDataRequiredinRoutineAnalysis日常分析析所需質(zhì)質(zhì)量數(shù)據(jù)據(jù)DataRequired所需數(shù)據(jù)I.D.名稱ImpurityTesting雜質(zhì)檢測(cè)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(cè)限NONONONOQuantitationlimit定量限NOMAYBENOMAYBELinearity線性NOYESNOYESRange范圍NONONONO1–mayberequiredwhenworkinginunknownmatrix40ReviewofQualityAssurance質(zhì)量保證證概述Wewillcover（內(nèi)容）DefinitionandDescriptionofQA質(zhì)量保證證的定義義和描述述ToolsinaQASystem（QA體系的工工具）ProficiencyTesting（能力驗(yàn)證證）CertifiedReferenceMaterials（有證標(biāo)準(zhǔn)準(zhǔn)物質(zhì)））ValidatedMethods（經(jīng)過確認(rèn)認(rèn)的方法法）41QualityAssurance（質(zhì)量保證證）QualityAssurance質(zhì)量保證證Plannedactionsdesignedtoprovideconfidencethatqualityrequirementswillbefulfilled為質(zhì)量要求得得到滿足提供供信心而設(shè)計(jì)計(jì)的有計(jì)劃的的活動(dòng)QualityAssuranceSystem質(zhì)量保證體系系A(chǔ)setofprocessesappliedwithinadefinedstructuretogeneratedesiredoutcomes在規(guī)定的結(jié)構(gòu)構(gòu)內(nèi)產(chǎn)生預(yù)期期結(jié)果所采用用的一組過程程Thegoodmanagementofgoodscience良好的科學(xué)良良好的管理42QualitySystemComponents質(zhì)量體系組成成Management管理Plan策劃Performance實(shí)施Do做Assessment評(píng)價(jià)Review評(píng)審436PillarsofQA/QC

QA/QC的六個(gè)基礎(chǔ)Management管理Facilities設(shè)施Personnel人員CRM’s有證標(biāo)準(zhǔn)物質(zhì)質(zhì)PT’s能力驗(yàn)證ValidatedMethods經(jīng)確認(rèn)的方法法44ProficiencyTesting能力驗(yàn)證Providesexternalassessmentofperformance為表現(xiàn)提供外外部評(píng)審Providesabasisforcorrectiveandpreventiveaction為糾正和預(yù)防防措施提供基45InformationGained搜集信息Comparisonofperformanceagainstanexternalstandard將表現(xiàn)與外部部標(biāo)準(zhǔn)比較Comparisonagainstpastperformance與過去的表現(xiàn)現(xiàn)比較Comparisonagainstpeer(competitor)labs與同行（競爭爭者比較）Identificationofunsatisfactoryperformers識(shí)別出不滿意意的操作者46TypesofPT能力驗(yàn)證類型型Specificanalyte/matrixcombination特定被分析物物/基體結(jié)合合Mercuryinfish（（魚中的汞）Benzeneinair（空氣中的苯））Fieldofanalysis（場(chǎng)地分析）MetalsbyICP（ICP測(cè)金屬）PesticidesbyGC/MS（GC/MS測(cè)殺蟲劑）47Samples樣品Sub-sampledfrombulksupply從批中抽取樣樣本Discretesamplesplitanddistributed謹(jǐn)慎分割樣品品并分發(fā)48InterlaboratoryComparisons實(shí)驗(yàn)室間比對(duì)對(duì)Collaborativestudies協(xié)同研究Certificationstudies認(rèn)證研究Round-robinstudies循環(huán)研究49SelectionofPTprogramsPT方案的選擇Availabilityofrelevantprograms是否有相關(guān)方方案Organizationofrelevantprograms相關(guān)方案的組組織Anyprogramisusuallybetterthannothing只有要方案，，總比沒有好好50AssessmentofPTProgramsPT方案的評(píng)價(jià)Beforecommittinglong-termconsider在實(shí)施前應(yīng)考考慮Statisticsusedtointerpretdata解釋結(jié)果的統(tǒng)統(tǒng)計(jì)技術(shù)How“true”valueisdetermined真值如何確定定Theoretical理論值Refereelab參考實(shí)驗(yàn)室Consensus公議值51ScoringofParticipants參加者的評(píng)價(jià)價(jià)Z–score（Z值）Deviationfrom““true””valuedividedbysigma測(cè)得值與真值值之差除以σSigmamaybeanaccepteddeviationorstatisticallydeterminedineachroundσ可能是可接受受的偏差或每每輪測(cè)試的統(tǒng)統(tǒng)計(jì)結(jié)果52Scoring

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53LaboratoryInterpretation實(shí)驗(yàn)室的解釋釋Viewresultsincontext（從整體上看結(jié)結(jié)果）Dotheyagreewithin-houseQCdata是否與室內(nèi)質(zhì)質(zhì)量控制數(shù)據(jù)據(jù)一致Trendanalysis(considerhowsigmaisdetermined)趨勢(shì)分析（考考慮σ是如何確定的的）Performanceofotherparticipants其它參加者的的表現(xiàn)54LaboratoryInterpretation實(shí)驗(yàn)室的解釋釋Comparemethodologyandre-calculateifpossible比較方法，如如果可能重新新計(jì)算Compareuncertaintyagainstin-houseestimates將不確定度與與室內(nèi)評(píng)估比比較55CorrectiveActions糾正措施Determinewhentotakeaction確定何時(shí)采取取措施After1unsatisfactoryscore?一個(gè)不滿意結(jié)結(jié)果Aftermany(3)inoneround?一輪中多個(gè)（（如三個(gè)）不不滿意結(jié)果After2consecutiveunsatisfactoryscores?連續(xù)二個(gè)不滿滿意結(jié)果56CorrectiveActions糾正措施Alwaysinvestigate總要調(diào)查Include包括QCdata質(zhì)量控制數(shù)據(jù)據(jù)Calculations,dilutions,transcriptions計(jì)算、稀釋，，抄寫Trainingstatusofanalyst分析人員培訓(xùn)訓(xùn)狀況Performancerecordsofequipment設(shè)備運(yùn)行記錄錄Recordsofcalibrants,reagentsetc.校準(zhǔn)品、試劑劑的記錄等57CorrectiveActions糾正措施Formulateaction公布措施Executeaction實(shí)施措施Checkifactionwassuccessful檢查措施是否否有效58GeneralConsiderations幾點(diǎn)考慮MoreemphasisisbeingplacedonPTprogramsbyassessors,regulatorsandclients評(píng)審員、管理理部門和客戶戶更多強(qiáng)調(diào)PTUsealltheinformationavailable利用所有可得得到的信息HandlePT’slikeroutinesamples(asmuchaspossible)象常規(guī)樣品一一樣處理PT樣品（盡可能能）59ThirdPartyAssessment第三方評(píng)審AccreditationBodies認(rèn)可機(jī)構(gòu)AssessperformanceagainstlaboratoryscoperatherthanPTprogramcriteria在一定范圍圍內(nèi)評(píng)審實(shí)實(shí)驗(yàn)室的表表現(xiàn)，而不不是PT方案準(zhǔn)則Consider““fitforpurpose”考慮適宜性性60ThirdPartyAssessment第三方評(píng)審審Regulators政府管理部部門MaybeinvolvedindevelopmentofPTprograms可能參與PT方案的開發(fā)發(fā)Mayrequireassistancefromprogramcoordinatortoassessresults可能需要方方案協(xié)調(diào)人人來幫助評(píng)評(píng)審結(jié)果61ThirdPartyAssessment第三方評(píng)審審Customers客戶WhenusingPTresultsasaperformancestandardensuretargetisrealistic當(dāng)使用PT結(jié)果作為能能力標(biāo)準(zhǔn)時(shí)時(shí)，確保目目標(biāo)是現(xiàn)實(shí)實(shí)的Mustinvestigateprogram;notjustresults必須調(diào)查方方案，而不不僅是結(jié)果果62ReferenceMaterials參考物質(zhì)5types（5種類型）Puresubstance（純物質(zhì)）Standardsolutionsandgasmixtures（標(biāo)準(zhǔn)溶液和和氣體混合合物）MatrixRM’s（基體參考物物質(zhì)）Physicalproperties（物理特性））Referenceobjects(artifacts)（參考目標(biāo)））（參考品品）63ReferenceMaterials參考物質(zhì)Maybeusedfor可用于InternalQC內(nèi)部質(zhì)量控控制Methodvalidation方法確認(rèn)Calibration校準(zhǔn)Estimatinguncertainty評(píng)估不確定定度Training培訓(xùn)64Classification分類CertifiedReferenceMaterials有證參考物物質(zhì)Directlytraceable直接溯源Eachpropertyhasanuncertaintyassociatedwithit每一特性有有相應(yīng)不確確定度Referencematerial參考物質(zhì)Propertiesarehomogenousandthoroughlycharacterizedtobeusedforcalibrationormethodassessment特性是均勻勻的，并完完整定值，，以用于校校準(zhǔn)或方法法評(píng)價(jià)65Availability可獲得性Generallypoorthereforeexpensive(不容易獲得得,費(fèi)用高高)Governmentagencies政府機(jī)構(gòu)NIST,NRC,EU-BCRTradeassociations貿(mào)易易協(xié)協(xié)會(huì)會(huì)AOAC,AOCA(OilChemists)石油油化化學(xué)學(xué)Commercialsuppliers商業(yè)業(yè)供供貨貨商商66RMinValidation方法法確確認(rèn)認(rèn)中中參參考考物物質(zhì)質(zhì)的的使使用用Estimationofbiasbetweenmethodandtruevalue評(píng)估估方方法法和和真真值值間間的的偏偏差差Estimationo