GLP(良好實(shí)驗(yàn)室規(guī)范)

GLP(良好實(shí)驗(yàn)室規(guī)范)國家為了保證藥品的質(zhì)量安全制定的一系列規(guī)范，包括：GAP——中藥材生產(chǎn)質(zhì)量管理規(guī)范

GMP——藥品生產(chǎn)質(zhì)量管理規(guī)范

GLP——藥物非臨床研究質(zhì)量管理規(guī)范

GCP——藥物臨床試驗(yàn)管理規(guī)范（GoodClinicalPractice）GSP——藥品經(jīng)營質(zhì)量管理規(guī)范GUP——藥品使用質(zhì)量管理規(guī)范這些嚴(yán)格的規(guī)范被逐漸應(yīng)用到其它相關(guān)領(lǐng)域，尤其是食品行業(yè)：GAP（GoodAgriculturalPractice）:良好農(nóng)業(yè)規(guī)范GMP（GoodManufacturingPractices）:良好操作規(guī)范GLP（GoodLaboratoryPractice）:良好實(shí)驗(yàn)室規(guī)范GSP（GoodSupplyingPractice）：良好經(jīng)營（供應(yīng)）規(guī)范1hGLP(良好實(shí)驗(yàn)室規(guī)范)GLP是英文GoodLaboratoryPractice的縮寫，中文直譯為良好實(shí)驗(yàn)室規(guī)范。GLP是就實(shí)驗(yàn)室實(shí)驗(yàn)研究從計(jì)劃、實(shí)驗(yàn)、監(jiān)督、記錄到實(shí)驗(yàn)報(bào)告等一系列管理而制定的法規(guī)性文件，涉及到實(shí)驗(yàn)室工作的所有方面。它主要是針對醫(yī)藥、農(nóng)藥、食品、食品添加劑、化妝品、獸藥等進(jìn)行的安全性評價(jià)實(shí)驗(yàn)而制定的規(guī)范。制定GLP的主要目的是嚴(yán)格控制化學(xué)品安全性評價(jià)試驗(yàn)的各個(gè)環(huán)節(jié)，即嚴(yán)格控制可能影響實(shí)驗(yàn)結(jié)果準(zhǔn)確性的各種主客觀因素，降低試驗(yàn)誤差，確保實(shí)驗(yàn)結(jié)果的真實(shí)性。

2hGLP(良好實(shí)驗(yàn)室規(guī)范)

GLP始于20世紀(jì)70年代。新西蘭是第一個(gè)建立實(shí)驗(yàn)室登記法的國家。1976年美國食品藥品管理局（FDA）制定了僅限于藥品的GLP規(guī)范草案。1980年由美國聯(lián)邦環(huán)保局（EPA）在《聯(lián)邦殺蟲、殺菌、殺鼠劑法》中發(fā)布了有關(guān)農(nóng)藥的GLP標(biāo)準(zhǔn)。加拿大、日本、韓國等國家先后發(fā)布了本國的GLP法規(guī)。歐共體在1975年5月公布了關(guān)于藥品藥理毒理、臨床及臨床標(biāo)準(zhǔn)草案法規(guī)，在1986年提出GLP草案，1988年又發(fā)布GLP檢查法令。歐共體GLP與經(jīng)濟(jì)合作與發(fā)展組織（OECD）的GLP原則一致。1993年12月我國原國家藥品監(jiān)督管理局頒布了“藥品非臨床研究質(zhì)量管理規(guī)定”(試行)。國家環(huán)境保護(hù)總局等部委也先后制定了本行業(yè)的GLP標(biāo)準(zhǔn)。我國農(nóng)藥行業(yè)GLP工作始于2002年。3hGLP(良好實(shí)驗(yàn)室規(guī)范)CONTENTS內(nèi)容1、整潔有序的實(shí)驗(yàn)室日常管理GOODHOUSEKEEPINGPRACTICE2、安全規(guī)范SAFETYPRACTICE3、符合專業(yè)要求的操作GOODOPERATIONALPRACTICE4、純凈水PURIFIEDWATER5、標(biāo)準(zhǔn)物質(zhì)REFERENCEMATERIALS6、標(biāo)準(zhǔn)溶液STANDARDSOLUTIONS7、留樣RETAINEDSAMPLES8、實(shí)驗(yàn)室器皿的清潔CLEANINGOFLABORATORYWARE9、化學(xué)通風(fēng)櫥FUMECUPBOARDS10、層流通風(fēng)柜（超凈工作臺(tái)）LAMINARFLOWHOODS11、實(shí)驗(yàn)室能力驗(yàn)證LABORATORYPROFICIENCYTEST4h現(xiàn)場的5S??！GLP(良好實(shí)驗(yàn)室規(guī)范)1、GOODHOUSEKEEIPNGPRACTICE

整潔有序的實(shí)驗(yàn)室日常管理Workflow:Awellorganizedlaboratoryshouldminimizetheamountofbacktrackingandretracingofsteps.工作流程：實(shí)驗(yàn)室的布置應(yīng)合理有序，以有助于提高工作效率。Labsshallbekeptcleanandtidyandfreefromunnecessaryclutterandequipment.實(shí)驗(yàn)室應(yīng)保持清潔，整齊，不放置不需要的物品和儀器。Allgangways,aislesandexitswillbefreetoalloweasyaccess.通道，走廊和出口保持通暢。Allequipment,glasswareandothersupportinginstrumentationwillbebackintheirproperplaceafteruse.所有儀器，玻璃器皿和輔助器具使用后應(yīng)放加原處。Alabelwillbeplacedoneachcupboardanddrawtoidentifyitscontents.櫥柜和抽屜應(yīng)有標(biāo)識。Mostchemicalsinthelaboratoryarepotentiallyhazardous,theyshallbeproperlylabeledandseparatelystored.化學(xué)品應(yīng)分類存放，并按性質(zhì)作危害性標(biāo)識。5h現(xiàn)場的EHS！！GLP(良好實(shí)驗(yàn)室規(guī)范)2、SAFETYPRACTICE-1安全規(guī)范Personnelwillweardurableclothingthatcoversthearms,legs,torsoandfeet.Open-todeshoesandsandalswillnotbeworn.實(shí)驗(yàn)室人員應(yīng)穿著牢固的能遮蓋手臂、腿、身體和腳的服裝，不得穿著露趾鞋和拖鞋。Aclean,fastenedcottonlaboratorycoatwillbeworn.Laboratorycoatswillnotbeworninrefreshmentareasorlunchrooms.應(yīng)穿著緊身的棉質(zhì)工作服，工作服不可穿進(jìn)茶點(diǎn)休息區(qū)域或食堂。Eyeprotectionwillbewornunlesstheanalystcandemonstratethatadequateprotectionisprovidedbyothermeans.實(shí)驗(yàn)室應(yīng)配備保護(hù)眼睛的設(shè)施，否則應(yīng)配戴護(hù)眼鏡。Eachlaboratoryhasdedicatedhandwashingfacilities-includingsoapandpapertowels.Handsarewashedonenteringthelaboratorybeforestartinganalysis,andwhenenteringandexitingthelaboratoryforlunchorgoingtothetoilet.實(shí)驗(yàn)室應(yīng)配備專用洗手設(shè)施-包括清潔劑和紙巾。進(jìn)入實(shí)驗(yàn)室開始分析前，離開實(shí)驗(yàn)室進(jìn)餐廳和由餐廳回實(shí)驗(yàn)室，或去洗手間均須洗手。6h現(xiàn)場的EHS！！GLP(良好實(shí)驗(yàn)室規(guī)范)2、SAFETYPRACTICE-2安全規(guī)范Appropriateglovesarewornwhenhandlingsubstancesthatmaybeabsorbedthroughtheskinorthatarecorrosive,harmfulormayirritatetheanalyst.處理易被皮膚吸收或腐蝕有害或刺激性的物質(zhì)時(shí)應(yīng)帶適當(dāng)?shù)氖痔?。Charactersofchemicals,suchas“Flammable”,“Corrosive”etc.shallbecorrectlyidentifiedandlabeled.化學(xué)品的特性，如“易燃”，“腐蝕”等應(yīng)正確標(biāo)識。Cylindersshallbefixedandclearlylabeled.鋼瓶應(yīng)清楚標(biāo)識，并固定。Cutsandgrazestotheskinareadequatelycoveredbysuitabledressings.傷口和皮膚擦破處應(yīng)適當(dāng)?shù)匕蠊?。Personnelwillnotworkinalaboratoryalone.不可單獨(dú)在實(shí)驗(yàn)室工作。Eating,drinkingandsmokingareprohibitedinthelaboratoryatalltimes.任何時(shí)候均不得在實(shí)驗(yàn)室吃、喝和抽煙。7hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-1

符合專業(yè)要求的操作-試劑的使用與配制-1Solventbottlesarealwayscoveredastheywillreadilyabsorbmoistureandcontaminantsfromtheair.溶劑易吸收空氣中的水分和污染物，溶劑瓶必須隨時(shí)蓋緊。Apipettewillnotbeusedtopipettedirectlyfromthebottleunlessitisanautomaticpipette.Theremainingsolventisnotreturnedtothestockbottle.Itmustbetreatedaswaste.不可用移液管直接從瓶中移取溶劑或溶液，應(yīng)傾倒入容器內(nèi)移取，剩余溶劑不可倒回貯液瓶，應(yīng)作廢棄物處理。Aspatulaorspoonwillnotbeplaceddirectlyintothebottleforsolids.Therequiredquantityisdecantedintoanothercontainerfromwhichthematerialwillberetrieved.Theremainingmaterialwillnotbereturnedtostockbottle.Itshouldbetreatedaswaste.不可用刮勺或匙直接從瓶中取用固體試劑，應(yīng)在另一容器中傾入所需量。剩余試劑不可倒回原容器，應(yīng)作廢棄物處理。8hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-2

符合專業(yè)要求的操作-試劑的使用與配制-2Laboratorypersonnelshallbemadeawareoftheirresponsibilitiesintheuseofsuitablereagents,solvents,culturemedia,referencematerialsandlaboratorywareintermsofthetypesofanalysistheyconduct.實(shí)驗(yàn)室人員應(yīng)明確其有責(zé)任根據(jù)所進(jìn)行的測試使用適合的試劑、溶劑、培養(yǎng)基、參照物和實(shí)驗(yàn)室器皿。Anypossiblecontamination,includingLeftoversthathasbeenreturnedtothecontainers.任何可能導(dǎo)致污染的操作，包括將取出未用完的試劑、溶劑、培養(yǎng)基、參照物放回容器，受影響的物質(zhì)均應(yīng)視為失效。INTEGRITYOFREAGENTSAllreagentcontainersshallbelabeledandtightlyclosed.Theyshallbeartheoriginallabel.所有試劑容器均應(yīng)標(biāo)識和蓋緊。容器上的標(biāo)貼必須為原標(biāo)貼。INTEGRITYOFREAGENTS9hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-3

符合專業(yè)要求的操作-試劑的使用與配制-3Thepersonresponsibleforthepreparationofthereagentshallbeidentifiableeitherfromthelabelorfromrecords.試劑的配制人應(yīng)在標(biāo)貼上標(biāo)識或在記錄中寫明。Laboratoryshallestablishwrittenproceduresforpreparationofreagentsolutionsandculturemedia.Recordsofsuchpreparationshallbemaintained.實(shí)驗(yàn)室應(yīng)建立試劑溶液和培養(yǎng)基配制方法的文件。應(yīng)保存配制記錄。Recordsforreagentsolutionsshallincludemeasuredweightsandvolume,burettereadings,pHreadings,calculationofstandardizationfactorandsolutionconcentration.試劑溶液配制記錄應(yīng)包括重量，體積，滴定管讀數(shù)，PH讀數(shù)標(biāo)定因子的計(jì)算和溶液濃度。10hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-4

符合專業(yè)要求的操作-試劑的使用與配制-4Thepreparationrecordforculturemediashallincludemediumname,batchnumber,amountprepared,pHbeforeandafterautoclavingautoclavetimeandpressure.培養(yǎng)基的配制記錄應(yīng)包括名稱、批號、配制量、壓熱鍋處理前后的PH值，處理時(shí)間和壓力。Wherelaboratorypreparesitsownmedia,thechemicalsusedforsuchpreparationshallbeverifiedtobeoftheappropriatequalitybeforeuse.如實(shí)驗(yàn)室自己制備培養(yǎng)基，使用前應(yīng)確認(rèn)所用化學(xué)品符合質(zhì)量要求?！癶azardoussubstance”shallbekeptseparatelyfromotherreagentsandheldinlockedcabinets.危險(xiǎn)物質(zhì)應(yīng)與其它試劑分別存放，并加鎖。11hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-5

符合專業(yè)要求的操作-試劑的使用與配制-5PreparationAndStorageOfCulturemedia培養(yǎng)基的制備和存儲(chǔ)Culturemediamustbepreparedandstoredatthespecifiedtemperatureandunderthespecifiedconditionsaccordingtothemanufacturer’sinstructionsormethodrequirements.Eachlotofpreparedorpurchasedculturemediamustverifiedforitseffectiveness.培養(yǎng)基必須按照制造商的說明或方法要求在規(guī)定的溫度和條件下制備和存放。無論是購買的或制備的培養(yǎng)基，其有效性必須驗(yàn)證。PreparedPlatesofCultureMedia:PouredplatesofagarMediaareespeciallyvulnerabletoinfection,dehydrationandchemicaldegradation.Asepticpreparationandstorageareessentialtoprotectplatesfrommicrobialinfection.培養(yǎng)基制備平板，例如瓊脂傾注平板，特別易受微生物侵染，脫水，和化學(xué)降解，為使平板不受微生物侵染，必須進(jìn)行無菌制備和存放。12hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-6

符合專業(yè)要求的操作-試劑的使用與配制-6GR(Guaranteedreagents)保證試劑（優(yōu)級純）（一級）綠色AR(Analyticalreagents)分析純（二級）紅色CP(Chemicalpure)化學(xué)純（三級）藍(lán)色LR(Laboratoryreagents)實(shí)驗(yàn)試劑（四級）中黃色CorrectlySelectReagents正確選用試劑GR:用于精密度和準(zhǔn)確度較高的分析AR:用于常規(guī)分析工作CP:通常不用于分析工作，尤其不適合配制標(biāo)準(zhǔn)溶液LP:不適合用于分析工作此外，有特定用途的試劑純度有高純試劑，如光譜純、色譜純等。ARcanbeusedforpreparingstandardsolutionsbutnotforstandardization.分析純試劑可用于配制標(biāo)準(zhǔn)溶液，但不可用于標(biāo)定。13hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-7

符合專業(yè)要求的操作-稱量過程-1Glassvesselsusedtoweighmaterialwillnotbewipedwithadryclothasthiscausesstaticelectricitybuildupinthecontainer.Donotputmaterialtobeweighedintheweighingdishmorethan2/3ofitsvolume.用于稱量樣品或試劑的玻璃器皿不可用干織物擦試以免產(chǎn)生靜電。樣品不能超過稱量皿體積的2/3。Allsamplesandcontainersareatthesametemperatureastheweighingdevice.Therefore,allmaterialsareallowedtoequilibratetoroomtemperaturepriortouse.所有樣品和容器應(yīng)與稱量裝置置于同一溫度，以使所有物料使用前在室溫下平衡。Allweighingdevicesarecalibratedorverifiedpriortouse.Verificationshallbeconductedat?and2timesoftargetvalue.稱量儀器使用前應(yīng)校驗(yàn)或驗(yàn)證，驗(yàn)證應(yīng)在1/2及2倍目標(biāo)稱量值處進(jìn)行。14hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-8

符合專業(yè)要求的操作-稱量過程-2Barehandcannevertouchtheweights,cleanglovesshouldbeworn.不可用手接觸砝碼，應(yīng)佩戴干凈手套。Ovenshouldbeequilibratedatspecifiedtemperaturepriortotestingthelossofweightondrying.Sampleafterdryingshallbecooledforafixedandconstanttimeinterval.進(jìn)行干燥失重測試前，應(yīng)先將烘箱開啟在規(guī)定溫度下達(dá)到平衡。干燥后樣品的冷卻時(shí)間應(yīng)恒定。Properlyplaceobjectsbeingdriedinthedesiccator,nostackingisallowed.在干燥器中的物體不可疊放。15hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-9

符合專業(yè)要求的操作-容量器具的使用-1Theuseofdryingsolvents(e.g.acetone),compressedairandpapertowelswillbeavoided,wherepossible,asthesemaybeothersourcesofdamageorcontamination.盡可能避免使用干燥溶劑（如丙酮），壓縮空氣和紙巾以免可能的損壞或污染。Glassstopperspurchasedwiththevolumetricflaskswillremainwiththatflask.容量瓶的玻璃塞須保持原配。Useofpipettes:thesolutionsarenotmouthpipettedirrespectiveoftheirnature.任何溶液均不可用移液管通過嘴吸取。Allpipettesareinspectedcarefullypriortouse.Itwillbecheckedforcracksinthetip;ifpresentitwillbediscarded.Pipettesarecleananddrypriortouse.移液管在使用前應(yīng)檢查頂端是否有裂紋；移液管使用前必須清潔干燥。16hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-10

符合專業(yè)要求的操作-容量器具的使用-2Thepipetteisrinsedatleasttwicewiththesamplesolutionbeforeuse.移液管使用前應(yīng)至少用樣品溶液潤洗兩次。Whenremovingsolutionfromaflask,sufficientvolumeisdrawntoslightlyabovethemark,thesolutionisallowedtodrawdowntothemarkbytouchingthetipofthepipettetotheflasksurface.Anyexcessfluidfromthepipetteiswipedinadownwardmotionthenthealiquotisdelivered.當(dāng)由容量瓶移出溶液時(shí)，溶液體積應(yīng)略高于刻度，然后用移液管尖端接觸溶量瓶表面的方法將溶液調(diào)節(jié)至刻度。Note:mostpipettesaredesignednottobeexpelled(i.e.liquidshouldremaininthetipafteruse).多數(shù)移液管都無須將殘留液趕了（即將殘留液留在移液管尖端）。Volumetricglasswarecannotbekeptinheatingenvironment,orinrefrigeratororcoolingcabinet.Donotholdthequantitativepartofthevolumetricglasswarewithhand.所有容量器具不能存放在加熱環(huán)境下或冰箱內(nèi)。使用時(shí)不能用手捂住容量部分。17hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-11

符合專業(yè)要求的操作-容量器具的使用-3Graduatedmeasuringcylindersarereadbyplacingthemonanevenbench,andobservingthemeniscusateyelevel.Volumeisequivalenttothebottomofthemeniscus.刻度量筒放置于平坦的桌面上讀數(shù)，視線應(yīng)與彎月面同一水平，由彎月面底部讀取體積。Itemssuchasbeakers,Erlenmeyerflasksandotherglasswarewithrudimentaryvolumemarkingswillnotbeusedformeasuringvolume.帶有粗刻度的器皿，如燒杯、三角瓶等玻璃器皿不可用于量度體積。Allvolumetricglasswareshallbeverifiedbeforeuse;Pipettesshallbeverifiedonceevery3month,andautopipettesverifieddailybeforeuse,recordquarterly;Whethervolumetricflaskisverifiedquarterlyshallbebasedonuncertaintycontribution.Allverificationisrecorded.所有容量器具使用前必須經(jīng)過驗(yàn)證。移液管每三個(gè)月驗(yàn)證一次，移液槍每次使用前驗(yàn)證，并每三個(gè)月記錄一次。容量瓶的驗(yàn)證根據(jù)它對方法結(jié)果的不確定度貢獻(xiàn)在方法的SOP中注明是否需要每三個(gè)月驗(yàn)證一次。所有驗(yàn)證均須記錄。18hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-12

符合專業(yè)要求的操作-容量器具的使用-4Allmeasurableglassware,suchaspipetteandvolumetricflask,shouldbeverifiedwithcertifiedthermometer,weightsshouldalsobecertifiedandincalibrationstatus.容量器皿（如移液管和容量瓶）的驗(yàn)證應(yīng)使用處理校驗(yàn)狀態(tài)的有證溫度計(jì)及砝碼.Volumetricmeasurementisanessentialelementinananalyticallaboratoryasmanytypesofdeterminationrequirespecificdilutionsandquantitativedeliveryofsolutions.容量分析是分析實(shí)驗(yàn)室的基本內(nèi)容，因?yàn)樵S多測試均涉及定量稀釋和溶液的定量轉(zhuǎn)移。Regardlessoftypeofvolumetricglassware,whereaccuracyisrequired,especiallyforquantitativeanalysis,allofsuchvolumetricequipmentshallbecalibrated.容量儀器應(yīng)恰當(dāng)?shù)鼐S護(hù)和檢查，任何容量分析玻璃器皿,只要有精確度的要求，尤其是定量分析，所有這些儀器均應(yīng)進(jìn)行校驗(yàn)。19hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-13

符合專業(yè)要求的操作-容量器具的使用-5Coca-colarequiresthat“classA”glasswareshallbeusedforvolumetricanalysis.Doesthismeannocalibrationisnecessaryforanyglasswaremarked“A”?可口可樂系統(tǒng)規(guī)定使用”A“級容量器皿，這是否意味著凡是標(biāo)識”A“的容量器皿都不必要校驗(yàn)？甚至使用了十余年也無需驗(yàn)證其是否仍符合A級要求嗎？IsyourClassAglasswaresuppliedwithaserializedcertificateofprecision?你的”A“級容量器皿有不重復(fù)編號的效證書嗎？GlassAglasswareneedonlybeusedwheresuchvolumetricaccuracyiscriticaltotheperformanceofthemethodand,whereitisrequired,theglasswaremustbecalibratedasconformingtoClassAtolerance.A級玻璃器皿僅在容量準(zhǔn)確性對方法結(jié)果而言為必須時(shí)才使用，當(dāng)需要用A級時(shí)，必須校驗(yàn)以確認(rèn)符合A級的容許誤差。20hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-14

符合專業(yè)要求的操作-容量器具的使用-6Glasswareusedformeasuringsamples,standardsandreagentsforanalyticalproceduresmustbeClassA.用于測量進(jìn)行測試的樣品、標(biāo)準(zhǔn)和試劑的玻璃器皿必須是A級。AllplasticvolumetriccontainersareClassB.所有塑料容量分析容器均是B級。SyringesandautomatictippipettorsarenotlistedasClassA.注射器和自動(dòng)移液管不列為A級。21hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-15

符合專業(yè)要求的操作-樣品處理Samplepreparation:Allpreparationswillbedonetomininizethepotentialriskofcontaminationordegradingthematerialtobeanalyzed.樣品制備應(yīng)將待測物質(zhì)潛在的污染和降解或變質(zhì)可能性降至最小。22hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-16

符合專業(yè)要求的操作-記錄保存RecordingProfessionally.記錄保存應(yīng)符合規(guī)范。Logbookisusuallynotoriginalrecord.Adequateinformationandrawdata,suchascalculation,shallbemaintained.數(shù)據(jù)表通常并非原始記錄，記錄應(yīng)包含充分的信息及原始數(shù)據(jù)，例如計(jì)算。Recordshallbemadeatthetimewhentheactivityiscarriedout,neverdoitafterwards.確保記錄的實(shí)時(shí)性。避免任何形式的”補(bǔ)記“。23hGLP(良好實(shí)驗(yàn)室規(guī)范)3、GOODOPERATIONALPRACTICE-17

符合專業(yè)要求的操作-培訓(xùn)Anumberofextraneousconditionsmayinfluencetheprecisionofagivenmeasurement.Theyincludetemperature,methodofdelivery,depthofcolorofthesolution,typeofmeniscus,calibrationtocontainordeliveradefinitevolume,andsoforth.Thuspropertrainingofpersonnelandcontinuingobservationoftheiroperationsshallbeinstitutedaspartofthequalityassuranceprocesstominimizeoreliminateproblemsassociatedwiththeseextrinsicfactorswhichcanaffectpreciseliquidmeasurements.許多外部條件將影響測試的精確性，例如溫度，樣品或溶液的轉(zhuǎn)移方法，溶液顏色深度，液柱彎月面的形狀，確定體積的容量或轉(zhuǎn)移量的校驗(yàn)等。因此，恰當(dāng)?shù)娜藛T培訓(xùn)，操作的持續(xù)監(jiān)視應(yīng)成為實(shí)驗(yàn)室品質(zhì)保證過程的一部分，以減少或消除這些影響液體精確測量的外部因素。24hGLP(良好實(shí)驗(yàn)室規(guī)范)4、PURIFIEDWATER-1純凈水Purifiedwaterisoneofthemostcriticalbutmostoftenneglectedreagentsusedinlaboratoryoperations.Useofimproperlypurifiedwatermayaccountforthefailureofanalysis.水是最重要而常被忽視的試劑之一，使用不合格的水可能會(huì)導(dǎo)致分析的失敗。Distillationofwaterwillnotalwaysensurequality.Thematerialsandconstructionofthedistiller,andthecharacterofrawwaterallinfluencethequalityofthedistillate.Thestoragecontainer,too,cansignificantlyinfluencethepurityofthewater.蒸餾并不總能確保水的質(zhì)量，蒸餾裝置的材質(zhì)和構(gòu)造，以及原水的品質(zhì)均影響蒸餾水的質(zhì)量。儲(chǔ)存容器也將顯著地影響蒸餾水的質(zhì)量。25hGLP(良好實(shí)驗(yàn)室規(guī)范)4、PURIFIEDWATER-2純凈水Stillsneedperiodiccleaningtoremovescale.蒸餾裝置需定期清潔和除垢。Formorepreciseanalysis,itmaybenecessarytousewaterdistilledfromquartzorall-borosilicateglassdistillationsystem.要求較嚴(yán)格的分析可能需使用石英硼硅玻璃蒸餾裝置精餾的水。Purifiedwatercanbedefinedaswaterthathasbeendistilledand/ordeionizedsothatitmeetsrelevantstandardorspecifications.純凈水為經(jīng)蒸餾和/或去離子的水，以達(dá)到或高于相關(guān)的標(biāo)準(zhǔn)或規(guī)格。26hGLP(良好實(shí)驗(yàn)室規(guī)范)4、PURIFIEDWATER-3純凈水分析實(shí)驗(yàn)室用水國家標(biāo)準(zhǔn)一、二、三級實(shí)驗(yàn)室用水的技術(shù)指標(biāo)（GB6682-92)名稱一級二級三級PH值范圍（25℃）------5.0-7.5電導(dǎo)率（25℃），μS/cm.≤0.115可氧化物質(zhì)（以O(shè)2計(jì)），mg/L＜---0.080.4吸光度（254nm,1cm光程）≤0.0010.01---蒸發(fā)殘?jiān)?05℃±2℃），mg/L≤---1.02.0可溶性硅（以SiO2計(jì)），mg/L≤0.010.02---一級水用于有嚴(yán)格要求的分析實(shí)驗(yàn)，如液相色譜分析用水等。二級水用于無機(jī)痕量分析，如原子吸收光譜分析用水等。三級水用于一般的分析工作。27hGLP(良好實(shí)驗(yàn)室規(guī)范)4、PURIFIEDWATER-4純凈水Grade1watershouldbeproducedbyfurthertreatmentofgrade2water,forexamplebyreverseosmosisorionexchangefollowedbyfiltrationthroughamembranefilterofporesize0.2μmtoremoveparticlematterorre-distillationfromafusedsilicaapparatus.一級水可用二級水經(jīng)過石英設(shè)備蒸餾，或離子交換或反相滲透再經(jīng)0.2μm孔徑的薄膜過濾器處理獲得。Grade2watercanbeproducedbymultipledistillation.Re-distillationcanalsousesub-boilingsilicadistillationapparatus.二級水可用多次蒸餾或離子交換等制得，二次蒸餾水一般可達(dá)到二級標(biāo)準(zhǔn)。第二次蒸餾也可采用石英亞沸蒸餾器。Grade3watercanbeproducedbysingledistillation,byionexchange,orbyreverseosmosis.Unlessotherwisespecified,itshouldbeusedforordinaryanalyticalwork.三級水可用一次蒸餾，離子交換，或反相滲透制得。通常，三級水可用于普通的分析工作。28hGLP(良好實(shí)驗(yàn)室規(guī)范)5、REFERENCEMATERIALS-1標(biāo)準(zhǔn)物質(zhì)Definitions(定義)：ReferenceMaterial(RM):Amaterialorsubstance,oneormorepropertiesofwhicharesufficientlywellestablishedtobeusedforthecalibrationofapparatus,theassessmentofameasurementmethod,orforassigningvaluestomaterials.參照物（RM）：一種材料或物質(zhì)，其一項(xiàng)或多項(xiàng)物性值得到充分確定，用于校驗(yàn)儀器和評價(jià)測量方法或確定材料的性能值。CertifiedReferenceMaterial(CRM):Areferencematerial,oneormoreofwhosepropertyvaluesarecertifiedbyatechnicallyvalidprocedureaccompaniedbyortraceabletoacertificateorotherdocumentationwhichisissuedbyacertifyingbody.有證參照物（CRM)：一種材料或物質(zhì)，其一項(xiàng)或多項(xiàng)特性值通過采用技術(shù)上獲得認(rèn)可的方法并可溯源至認(rèn)可機(jī)構(gòu)頒發(fā)的證書或其它的文件而獲得認(rèn)證。29hGLP(良好實(shí)驗(yàn)室規(guī)范)5、REFERENCEMATERIALS-2標(biāo)準(zhǔn)物質(zhì)CertifiedReferencematerials有證基準(zhǔn)物Acertifiedreferencematerialcanbedefinedasahomogeneousmaterialwithspecificpropertiessuchasidentity,purity,andpotencythathasbeenmeasuredandcertifiedbyaqualifiedandrecognizedorganization.有證基準(zhǔn)物是經(jīng)有資質(zhì)并獲得承認(rèn)的機(jī)構(gòu)測定和鑒證的具有特定性質(zhì)，例如屬性、純度、強(qiáng)度的均勻物質(zhì)。注：中國國家標(biāo)準(zhǔn)將有證標(biāo)準(zhǔn)物質(zhì)為一級和二級Thesematerialsarequiteexpensiveandmayormaynotbeusedineverydayoperations.Theyareoftenusedto“calibrate”and/orassayso-called“workingorsecondaryreferencematerials.日常操作可使用經(jīng)有證基準(zhǔn)物標(biāo)定的”二次標(biāo)準(zhǔn)“。30hGLP(良好實(shí)驗(yàn)室規(guī)范)5、REFERENCEMATERIALS-3標(biāo)準(zhǔn)物質(zhì)Caremustbetakenforthecertifiedreferencematerialstoensurethattheyarepackaged,storedandhandledproperlytopreventdeterioration.Certificateandrecordsofreceiptanduseshallbemaintained.有證基準(zhǔn)物必須妥善包裝、存放和處置，以防止變質(zhì)，應(yīng)保存收貨和使用記錄及證書，計(jì)算時(shí)應(yīng)按證書標(biāo)明的含量。Thelaboratoryshallassignsuitablestaffasmonitor(s)forcertifiedreferencematerials.Theirdutiesshallincludeorderingorassistingintheorderingofnewreferencematerials,checkingcalculationsofassays,refillingemptyworkingsupplycontainers,keepinglistsoflaboratory-availablecertifiedreferencematerialsuptodate.指定合適人員監(jiān)控有證基準(zhǔn)物，其職責(zé)包括訂購或協(xié)助訂購的基準(zhǔn)物，檢查計(jì)算，向?qū)Ｓ玫目杖萜髦醒a(bǔ)充基準(zhǔn)物溶液，和更新實(shí)驗(yàn)室有證基準(zhǔn)物清單。31hGLP(良好實(shí)驗(yàn)室規(guī)范)5、REFERENCEMATERIALS-4標(biāo)準(zhǔn)物質(zhì)Itispreferabletokeepsign-inandsign-outlogbooks.Eachanalystusingacertifiedreferencematerialshallregisterthenameofthereferencematerial,thedateandtimeitistakenandreturned,andhisorherinitials.一個(gè)值得提倡的做法是設(shè)置一簽收和簽發(fā)記錄本。每個(gè)使用有證基準(zhǔn)物的分析員均登記基準(zhǔn)物名稱，取用和返還的日期和時(shí)間，以及使用者小簽。Analystsshallbeinstructedforthecareofcertifiedreferencematerialsandfollowingtheproceduresforhandlingthem.分析員必須了解并按有證基準(zhǔn)物的處置程序使用和處置有證基準(zhǔn)物。32hGLP(良好實(shí)驗(yàn)室規(guī)范)5、REFERENCEMATERIALS-5標(biāo)準(zhǔn)物質(zhì)WorkingReferenceMaterials工作標(biāo)準(zhǔn)（二次標(biāo)準(zhǔn)）Aworkingreferencematerialcanusuallybedefinedasasubstanceotherthanacertifiedreferencematerialthatisstandardizedwithcertifiedreferencematerialandusedasareferencematerialinday-to-dayanalyses.工作標(biāo)準(zhǔn)（二次標(biāo)準(zhǔn)）通常是采用有證基準(zhǔn)物進(jìn)行標(biāo)定用作日常分析工作的標(biāo)準(zhǔn)。Aworkingreferencematerialshallbeassayedbythebestmethodavailable,andtheresultsshallbeenteredinanotebookforthatpurpose.Entriesshallincludetheanalyst’sname,dateofanalysis,source,lotnumber,allrawdata,charts,andcalculations.工作標(biāo)準(zhǔn)（二次標(biāo)準(zhǔn)）應(yīng)用最好的方法標(biāo)定，結(jié)果記入專用記錄。記錄內(nèi)容包括分析員姓名、分析日期、基準(zhǔn)的來源和批號，所有原始數(shù)據(jù)、圖表和計(jì)算。33hGLP(良好實(shí)驗(yàn)室規(guī)范)5、REFERENCEMATERIALS-6標(biāo)準(zhǔn)物質(zhì)Aworkingreferencematerialshallbehandledinessentiallythesamemannerasacertifiedreferencematerial,andarecordshallbemadeeachtimethestandardiswithdrawnforuse.工作標(biāo)準(zhǔn)（二次標(biāo)準(zhǔn)）的處置方法與有證基準(zhǔn)物基本相同，每次取用均應(yīng)記錄。Re-assaysofworkingreferencematerialsshallbecarriedoutregularlytoensurecontinuedintegrity.工作標(biāo)準(zhǔn)（二次標(biāo)準(zhǔn)）應(yīng)定期重復(fù)標(biāo)定以確保其持續(xù)的完整性。34hGLP(良好實(shí)驗(yàn)室規(guī)范)5、REFERENCEMATERIALS-7標(biāo)準(zhǔn)物質(zhì)Astandardinchemistryisareliableandreadilyquantifiedsubstance.Featuresofastandardinclude:標(biāo)準(zhǔn)物質(zhì)是一種化學(xué)性質(zhì)可靠，易定量的物質(zhì)，標(biāo)準(zhǔn)物質(zhì)應(yīng)具備如下性質(zhì)：1.Highpurity高純度2.Stability(lowreactivity)穩(wěn)定3.Lowhygroscopicityandefflorescence低吸濕和低風(fēng)化性4.Highsolubility(ifusedintitration)高溶解性（若用于滴定）5.Highequivalentweight高克當(dāng)量35hGLP(良好實(shí)驗(yàn)室規(guī)范)6、STANDARDSOLUTIONS-1標(biāo)準(zhǔn)溶液Asolutionofknownmolaritywithsufficientaccuracyiscalledastandardsolution.Itsconcentrationisdeterminedbyaprocessknownasstandardization.標(biāo)準(zhǔn)溶液是已知準(zhǔn)確克分子濃度的溶液，其濃度通過標(biāo)定獲得。Standardisationshouldgenerallybeconductedseparatelybytwoanalysts(4paralleleach)toensurethevalidityandreliabilityofthesolution.TheRelativeStandardDeviationfortheindividualsshouldnormallybewithin0.15%,theRSDfortwoanalystsshouldnormallybewithin0.20%unlessotherwisestated.標(biāo)定溶液實(shí)行雙人復(fù)核制（四標(biāo)四復(fù)原則），第一標(biāo)定人標(biāo)定后，由另一人獨(dú)立操作復(fù)核標(biāo)定，如無特殊規(guī)定，單人相標(biāo)對標(biāo)準(zhǔn)偏差應(yīng)在0.15%以內(nèi),兩人相對標(biāo)準(zhǔn)偏差應(yīng)在0.20%以內(nèi)，否則應(yīng)重新進(jìn)行標(biāo)定。RSD=100SD/X-bar36hGLP(良好實(shí)驗(yàn)室規(guī)范)IN-CLASSEXERCISE6-1(思考題）

為什么要四標(biāo)四復(fù)?Paralleltestsshallbeperformedforthedatareportedforadequateconfidenceofthetestresults.除過程控制及其它特定情況外，應(yīng)進(jìn)行平行樣測試。Avoidtakingvalueofmal-operationprobability.避免誤用由誤操作產(chǎn)生的數(shù)據(jù)（過失誤差）Themoretestsaredoneinparalleltheclosertheaverageofthedataistothetruevalue.Inchemicalanalysis,2-4paralleltestsarenormallyrequired.平行測定次數(shù)愈多，平均值愈接近真實(shí)值。在化學(xué)分析中，對于同一試樣，通常要求平行測定2-4次。37hGLP(良好實(shí)驗(yàn)室規(guī)范)IN-CLASSEXERCISE6-1(思考題）Themoretestsaredoneinparalleltheclosertheaverageofthedataistotheruevalue.Why?為什么增加平行測定次數(shù)能減小隨機(jī)誤差？Aprompt:提示：Commoncausedeviationsarerandomlytwo-wayoccurred38hGLP(良好實(shí)驗(yàn)室規(guī)范)6、STANDARDSOLUTIONS-2標(biāo)準(zhǔn)溶液Allchemicallaboratoriesmaintaincertainstocksofstandardsolutions.Thepreparationandstandardisationofthesesolutionsshallbeassignedtospecificstaff,andadequaterecordsshallbemaintainedforeachsolution.標(biāo)準(zhǔn)溶液的配制和標(biāo)定由指定的專人負(fù)責(zé)。每一溶液均應(yīng)保存恰當(dāng)?shù)挠涗?。Informationshallbekeptinasuitablerecordbookandshallincludeidentityofthesolution,strength,methodofpreparation,standardisationcalculations,recheckofsolutionforinitialstrength,date,andinitialsofthemonitor.記錄所包含的信息包括名、濃度、配制方法、標(biāo)定計(jì)算，溶液濃度的復(fù)查、日期和標(biāo)定人或監(jiān)控人的小簽。39hGLP(良好實(shí)驗(yàn)室規(guī)范)6、STANDARDSOLUTIONS-3標(biāo)準(zhǔn)溶液Anadequateauthorityshallberesponsibleforreviewingthestandardizationanditscalculation,andapprovingtheuseofthestandardsolution.批準(zhǔn)人負(fù)責(zé)審核標(biāo)定記錄及計(jì)算結(jié)果，并批準(zhǔn)標(biāo)準(zhǔn)溶液的使用。Thelabelonthebottleofthestandardsolutionshallindicatetheidentityofthesolution,methodusedinstandardisation,molarity(orstrength)tothecorrectnumberofsignificantfigures,dateofpreparationand/ordateofstandardisation,dateofexpiry(ifapplicable)andinitialoftheindividualwhoisresponsibleforthestandardization.標(biāo)準(zhǔn)溶液瓶標(biāo)簽慶標(biāo)示溶液名稱，標(biāo)定方法，精密至正確有效數(shù)字的克分子濃度（或強(qiáng)度），配制和/或標(biāo)定日期，失效日期（如適用），和負(fù)責(zé)人標(biāo)定人員的小簽。40hGLP(良好實(shí)驗(yàn)室規(guī)范)6、STANDARDSOLUTIONS-4標(biāo)準(zhǔn)溶液標(biāo)

準(zhǔn)

溶

液保存期限（月）名

稱分子式濃度

各種酸標(biāo)液

氫氧化鈉氫氧化鉀乙醇液

硝酸銀

硫氰酸銨

高錳酸鉀

高錳酸鉀

溴酸鉀

碘

液

硫代硫酸鈉

硫代硫酸鈉

硫酸亞鐵

硫酸亞鐵

亞砷酸鈉

亞硝酸鈉

EDTA

NaOHKOHAgNO3NH4SCNKMnO4KMnO4KBrO3I2Na2S2O3Na2S2O3FeSO4FeSO4Na3AsO3NaNO2Na2H2Y各種濃度各種濃度0.1與0.50.10.10.10.050.10.10.10.050.10.050.10.1各種濃度320.25332131323310.53Re-standardizingorre-preparingshallbenecessaryuponthetimeintervalspecifiedinrelevantstandard,whereavailable.Thelefttablemaybereferencedinthecasethattheeffectivetimeintervalisnotstated.標(biāo)準(zhǔn)溶液須按相關(guān)標(biāo)準(zhǔn)或方法規(guī)定的期限重新配制或重新標(biāo)定，在沒有規(guī)定可特的情形下，可參考左表。41hGLP(良好實(shí)驗(yàn)室規(guī)范)6、STANDARDSOLUTIONS-5標(biāo)準(zhǔn)溶液Example:daterminetheconcentrationofBariumhydroxideusingstandardHydrochloricAcid例：用鹽酸標(biāo)準(zhǔn)液滴定氫氧化鋇Ba(OH)2(aq)+2HCl(aq)BaCl2(aq)+2H2O(l)1molBa(OH)2=2molHClMolBa(OH)2=2×molHCl×VolHCl/VolBa(OH)2Q:Howtodesigntheconcentrationofstandardsolutionandweightofsampleinordertoacquireanaccurateresult?為了獲得準(zhǔn)確的測定結(jié)果應(yīng)如何掌握樣品重量和標(biāo)準(zhǔn)溶液濃度？Onetransfer一次移液或滴定較大的滴定劑體積42hGLP(良好實(shí)驗(yàn)室規(guī)范)7、RETAINEDSAMPLES留樣Aretainedsampleisapartofthematerialoriginatingfromthesameconsignmentastheanalyticalsample,and/orthematerialusedfortheanalysis,wherenecessary.留樣是分析樣和/或在必要情形下用于分析的試劑的一部分。Retainedsampleshallbeproperlysealed,appropriatelyidentifiedandstoredunderappropriateconditionforaspecifiedperiodforfutureproblemtrackingincaseitisnecessary.留樣容器應(yīng)妥善封口和標(biāo)識，在恰當(dāng)?shù)拇娣艞l件下保存規(guī)定的時(shí)間，以備必要時(shí)進(jìn)行問題追溯。Theretentiontimewilldependonthestabilityandanylegalrequirementsoftheretainedsample.留樣保存時(shí)間取決一樣品穩(wěn)定性，或法規(guī)要求。43hGLP(良好實(shí)驗(yàn)室規(guī)范)8、CLEANINGOFLABORATORYWARE–1

實(shí)驗(yàn)室器皿的清潔Cleanlaboratoryware-glasswareandnon-glassware,suchaspolyethylene,polypropyleneandTeflonware,isanessentialpartoflaboratoryoperationsandavitalelementofthequalityassuranceprogram.實(shí)驗(yàn)室器皿，包括玻璃器皿、聚乙烯(PE)、聚丙烯(PP)和聚四氟乙烯（PTFE）器皿的清潔是實(shí)驗(yàn)室的基本操作，是品質(zhì)保證至關(guān)重要的部分。Eachlaboratoryshallestablishsoundcleaningproceduresforglasswareandnon-glassware.Cleaningmayrequireseveralsteps,and,wheneverpossible,cleaningshouldbeginimmediatelyaftertheapparatusisused.實(shí)驗(yàn)室應(yīng)建立有效的器皿清潔程序。器皿使用后應(yīng)立刻清潔。Organicresiduesmayrequiretreatmentwithachromicacidcleaningsolution,andfollowedbywateranddistilledwater.器皿的有機(jī)污漬可能需用鉻酸洗液清洗，再用水和蒸餾水沖洗。44hGLP(良好實(shí)驗(yàn)室規(guī)范)8、CLEANINGOFLABORATORYWARE–2

實(shí)驗(yàn)室器皿的清潔Apparatusshallbedriedandstoredunderconditionsthatwillnotallowittobecomecontaminatedwithdustorothersubstances.清潔過的器皿應(yīng)在不受塵埃和其它物質(zhì)污染的條件下干燥和存放。Glasswareusedformicrobiologicaltestingshallbesterilizedbyautoclaveorotherappropriatemeans.Detergentresiduechecksshallalsobeperformedtoensurethatglasswarearefreefromresidualbacteriostaticaction.用于微生物測試的玻璃器皿應(yīng)通過高壓滅菌器或其它合適的方法滅菌。檢查清洗劑殘留，以確保玻璃器皿無殘留抑菌作用。45hGLP(良好實(shí)驗(yàn)室規(guī)范)8、CLEANINGOFLABORATORYWARE–3

實(shí)驗(yàn)室器皿的清潔Checkofcleanliness:Agoodtestforcleanlinessistoallowwatertodrainfromtheitem;theabsenceofdiscretedropletsofwaterontheinteriorsurfaceindicatesaclean,grease-freeinterior.玻璃器皿清潔度的檢查：水流經(jīng)器皿或由器皿中排出后內(nèi)壁不掛水珠。Dryingofvolumetricglassware:Ifitisnecessarytodryanitemofvolumetricglasswarebeforeuse,thisshouldbedonebyeitherallowingtodrainatambienttemperature,orrinsingwithacetoneandthenallowingtodrain.容量分析玻璃器皿的干燥：容量分析玻璃器皿不可在烘箱中烘干。如有必要在使用前干燥，可瀝干或用純凈丙酮淋過后瀝干。46hGLP(良好實(shí)驗(yàn)室規(guī)范)9、FUMECUPBOARDS–1

化學(xué)通風(fēng)櫥Theexhaustairshallbedischargedinsuchamannerastominimizerecirculationofcontaminantsintothebuilding.Adequatemakeupairshallbeprovidedtoreplacetheexhaustair.通風(fēng)櫥廢氣應(yīng)以減少污染氣在建筑物內(nèi)循環(huán)的方法排放。應(yīng)有充分的新鮮空氣補(bǔ)充排出的廢氣。Alloperationswhichmaygenerateairbornecontaminantsshallbeconductedinsideafumecupboard.凡生產(chǎn)氣載污染物的操作均應(yīng)在通風(fēng)櫥中進(jìn)行。Nochemicalsorapparatusshallbestoredinthefumecupboard.通風(fēng)櫥內(nèi)不可存放化學(xué)品或儀器及裝置。Itemsplacedinorinfrontoffumecupboardcreatesairturbulence,thismayaffectthecaptureofcontaminants.Tolimitthisensurethatworkisconductedinth