溶液澄清度中国药典与欧洲药典

溶液澄清度中国药典与欧洲药典溶液澄清度中国药典与欧洲药典溶液澄清度中国药典与欧洲药典溶液澄清度中国药典：附录ⅨB澄清度检查法本法系在室温条件下，将用水稀释至一定浓度的供试品溶液与等量的浊度 标准 excel标准偏差excel标准偏差函数exl标准差函数国标检验抽样标准表免费下载红头文件格式标准下载 液分别置于配对的比浊用玻璃管(内径15～16mm，平底，具塞，以无色、透明、中性硬质玻璃制成)中，在浊度标准液制备5分钟后，在暗室内垂直同置于伞棚灯下，照度为1000lx，从水平方向察看、比较；用以检查溶液的澄清度或其污浊程度。除还有规定外，供试品溶解后应立刻检视。品种项下规定的“澄清”，系指供试品溶液的澄清度相同于所用溶剂，或未超过0.5号浊度标准液。“几乎澄清”则指供试品溶液的浊度介于0.5号至1号浊度标准液的浊度之间。浊度标准贮备液的制备称取于105℃干燥至恒重的硫酸肼1.00g，置100ml量瓶中，加水适量使溶解，必要时可在40℃的水浴中温热溶解，并用水稀释至刻度，摇匀，放置4～6小时；取此溶液与等容量的10%乌洛托品溶液混淆，摇匀，于25℃避光静置24小时，即得。本液置冷处避光保留，可在两个月内使用，用前摇匀。浊度标准原液的制备取浊度标准贮备液15.0ml，置1000ml量瓶中，加水稀释至刻度，摇匀，取适量，置1cm吸收池中，照紫外-可见分光光度法(附录ⅣA)，在550nm的波长处测定，其吸光度应在0.12～0.15范围内。本液应在48小时内使用，用前摇匀。浊度标准液的制备取浊度标准原液与水，按下 表 关于同志近三年现实表现材料材料类招标技术评分表图表与交易pdf视力表打印pdf用图表说话 pdf 配制，即得。本液应临用时制备，使用前充分摇匀。级号0.51234浊度标准5.010.030.050.0原液/ml2.50水/ml97.5095.090.070.050.0欧洲药典：ClarityanddegreeofopalescenceofliquidsVISUALMETHOD一般方法Usingidenticaltest-tubesofcolourless,transparent,neutralglasswithaflatbaseandaninternaldiameterof15-25mm,comparetheliquidtobeexaminedwithareferencesuspensionfreshlypreparedasdescribedbelow,thedepthofthelayerbeing40mm.Comparethesolutionsindiffuseddaylight5minafterpreparationofthereferencesuspension,viewingverticallyagainstablackbackground.ThediffusionoflightmustbesuchthatreferencesuspensionIcanreadilybedistinguishedfromwaterR,andthatreferencesuspensionIIcanreadilybedistinguishedfromreferencesuspensionI.在内径15～25mm，平底，无色、透明、中性玻璃管中，加入等量的供试溶液与浊度标准液，使液位的深度都为40mm，按如下所述方法进行比较。浊度标准液制备5分钟后，以色散自然光照射浊度标准溶液和供试溶液，在黑色背景下从垂直方向察看、比较澄清度或污浊程度。色散自然光必须较容易划分浊度标准溶液Ⅰ与水，液Ⅰ浊度标准溶液Ⅱ与浊度标准溶AliquidisconsideredclearifitsclarityisthesameasthatofwaterRorofthesolventusedwhenexaminedundertheconditionsdescribedabove,orifitsopalescenceisnotmorepronouncedthanthatofreferencesuspensionI.如果供试溶液的澄清、透明程度与水相同，或许与所用溶剂相同，或许其澄清度不超过Ⅰ号浊度标准溶液，那么可判断该溶液为澄清。Hydrazinesulfatesolution.Dissolve1.0gofhydrazinesulfateRinwaterRanddiluteto100.0mLwiththesamesolvent.Allowtostandfor4-6h.硫酸肼溶液：取1.0g硫酸肼溶于水，加水稀释至100.0ml，静置4～6小时。Hexamethylenetetraminesolution.Ina100mLground-glass-stopperedflask,dissolve2.5gofhexamethylenetetramineRin25.0mLofwaterR.乌洛托品（六亚甲基四胺）溶液：在100ml容量瓶中，以25.0ml水溶解2.5g乌洛托品。Primaryopalescentsuspension(formazinsuspension).Totheexamethylenetetraminesolutionintheflaskadd25.0mLofthehydrazinesulfatesolution.Mixandallowtostandfor24h.Thissuspensionisstablefor2months,provideditisstoredinaglasscontainerfreefromsurfacedefects.Thesuspensionmustnotadheretotheglassandmustbewellmixedbeforeuse.浊度标准贮备液：在寄存乌洛托品溶液的100ml容量瓶中，加25.0ml的硫酸肼溶液。混淆，静置24小时，贮存在无表面要求的玻璃容器中，可在2个月内使用。该浊度液不得黏附玻璃，用前必须充分摇匀。Standardofopalescence.Dilute15.0mLoftheprimaryopalescentsuspensionto1000.0mLwithwaterR.Thissuspensionisfreshlypreparedandmaybestoredforupto24h.浊度标准原液：取浊度标准贮备液15ml，加水稀释、定容至1000ml。该液临用前制备，至多保留24小时。Referencesuspensions.PreparethereferencesuspensionsaccordingtoTable2.2.1.-1.Mixandshakebeforeuse.浊度标准液：由浊度标准原液与水按表1-1配制,即得。本液应临用前配制。Table1.-1IIIIIIIVStandardof5.0mL10.0mL30.0mL50.0mLopalescenceWaterR95.0mL90.0mL70.0mL50.0mL表1.-1IIIIIIIV浊度标准液5.0mL10.0mL30.0mL50.0mL水95.0mL90.0mL70.0mL50.0mLTurbiditystandard.Theformazinsuspensionpreparedbymixingequalvolumesofthehydrazinesulfatesolutionandthehexamethylenetetraminesolutionisdefinedasa4000NTU(nephelometricturbidityunits)primaryreferencestandard.ReferencesuspensionsI,II,IIIandIVhavevaluesof3NTU,6NTU,18NTUand30NTUrespectively.Stabilisedformazinsuspensionsthatcanbeusedtopreparestable,dilutedturbiditystandardsareavailablecommerciallyandmaybeusedaftercomparisonwiththestandardspreparedasdescribed.浊度标准：乳光悬浊贮备液[硫酸肼溶液和乌洛托品（六亚甲基四胺）溶液以等量体积混淆定为4000NTU（比浊测定法的浊度单位）储备液比较标准.浊度标准液I,II,III和IV相应的NTU值分别是3NTU,6NTU,18NTU和30NTU。稳定的乳光悬浊贮备液可用于稀释制]备浊度标准，拥有现实的商业价值，也能够与上述的标准化制备进行较。Formazinhasseveraldesirablecharacteristicsthatmakeitanexcellentturbiditystandard.Itcanbereproduciblypreparedfromassayedrawmaterials.Thephysicalcharacteristicsmakeitadesirablelight-scattercalibrationstandard.Theformazinpolymerconsistsofchainsofdifferentlengths,whichfoldintorandomconfigurations.Thisresultsinawideassayofparticleshapesandsizes,whichanalyticallyfitsthepossibilityofdifferentparticlesizesandshapesthatarefoundintherealsamples.Duetoformazin’sreproducibility,scatteringcharacteristicsandtraceability,instrumentcalibrationalgorithmsandperformancecriteriaaremostlybasedonthisstandard.因福马尔肼拥有一些我们所希望的特性，所以它是一种特别优秀的浊度标准物。它能够从被测原料中频频制备。拥有所想要的光闪射校正标准化的物理特性。福马尔肼聚合物由不同长度的链组成，他们能够折成各样形状，应此能够剖析不同大小和形状的粒子。这一特性使得我们能够对现实样品中所拥有的不同大小及性状的粒子进行测定。由于。福马尔肼拥有可重复性、光散射性、可描述性、仪器校准可算和操作标准化的特性，使其成为了浊度标准物。instrumentalmethods仪器方法简介IntroductionThedegreeofopalescencemayalsobedeterminedbyinstrumentalmeasurementofthelightabsorbedorscatteredonaccountofsubmicroscopicopticaldensityinhomogeneitiesofopalescentsolutionsandsuspensions.2suchtechniquesarenephelometryandturbidimetry.Forturbiditymeasurementofcolouredsamples,ratioturbidimetryandnephelometrywithratioselectionareused.该仪器是根据污浊液和悬浊液亚显微镜光密度的不均一性来测量光的吸收或光的散射，即散射测浊法和透射测浊法。对于有色样品的浊度测试法，要用到比率透射比浊法和可选择比率的散射比浊法。Thelightscatteringeffectofsuspendedparticlescanbemeasuredbyobservationofeitherthetransmittedlight(turbidimetry)orthescatteredlight(nephelometry).Ratioturbidimetrycombinestheprinciplesofbothnephelometryandturbidimetry.Turbidimetryandnephelometryareusefulforthemeasurementofslightlyopalescentsuspensions.Referencesuspensionsproducedunderwell-definedconditionsmustbeused.Forquantitativemeasurements,theconstructionofcalibrationcurvesisessential,sincetherelationshipbetweentheopticalpropertiesofthesuspensionandtheconcentrationofthedispersedphaseisatbestsemi-empirical.经过投射光（投射比浊法）或散射光（散射比浊法）来测量混悬粒子的光散射效能。浊度比率联合了透射比浊法和散射比浊法二者的原理。透射比浊法和散射比浊法用于测量拥有轻微乳光的混悬液。必须使用在精准的条件下制得的标准混悬液。因为混悬液的光学性质与分别相的浓度之间的关系最多是一个半经验值，所以定量测定主要使用标准曲线法。Thedeterminationofopalescenceofcolouredliquidsisdonewithratioturbidimetersornephelometerswithratioselection,sincecolourprovidesanegativeinterference,attenuatingbothincidentandscatteredlightandloweringtheturbidityvalue.Theeffectissogreatforevenmoderatelycolouredsamplesthatconventionalnephelometerscannotbeused.因为溶液颜色会产生负扰乱，衰减入射光和散射光并降低浊度值，用比率透射浊度法和可选择比率的散射浊度法测定有色溶液的乳光。对于正好适度的有色样品，效果特别好，以至于惯例的浊度仪不再使用。Theinstrumentalassessmentofclarityandopalescenceprovidesamorediscriminatorytestthatdoesnotdependonthevisualacuityoftheanalyst.Numericalresultsaremoreusefulforqualitymonitoringandprocesscontrol,especiallyinstabilitystudies.Forexample,previousnumericaldataonstabilitycanbeprojectedtodeterminewhetheragivenbatchofdosageformulationoractivepharmaceuticalingredientwillexceedshelf-lifelimitspriortotheexpirydate.用仪器来判断澄清度和乳光，试验所提供的分辨能力更强，不再依靠剖析者的视觉敏锐性来判断。对于定性监控和过程控制，特别是稳定性研究，数字化结果更有用。比如，以前所得的对于稳定性的数字化资料用于判断一个给定批号的剂量成分或活性药物组分是否超过了贮存期限或许没过有效期。NephelometryWhenasuspensionisviewedatrightanglestothedirectionoftheincidentlight,thesystemappearsopalescentduetothereflectionoflightfromtheparticlesofthesuspension(Tyndalleffect).Acertainportionofthelightbeamenteringaturbidliquidistransmitted,anotherportionisabsorbedandtheremainingportionisscatteredbythesuspendedparticles.Ifmeasurementismadeat90tothe°lightbeam,thelightscatteredbythesuspendedparticlescanbeusedforthedeterminationoftheirconcentration,providedthenumberandsizeofparticlesinfluencingthescatteringremainconstant.Thereferencesuspensionmustmaintainaconstantdegreeofturbidityandthesampleandreferencesuspensionsmustbepreparedunderidenticalconditions.TheTyndalleffectdependsuponboththenumberofparticlesandtheirsize.Nephelometricmeasurementsaremorereliableinlowturbidityranges,wherethereisalinearrelationshipbetweennephelometricturbidityunit(NTU)valuesandrelativedetectorsignals.Asthedegreeofturbidityincreases,notalltheparticlesareexposedtotheincidentlightandthescatteredradiationofotherparticlesishinderedonitswaytothedetector.Themaximumnephelometricvaluesatwhichreliablemeasurementscanbemadelieintherangeof1750-2000NTU.Linearitymustbedemonstratedbyconstructingacalibrationcurveusingatleast4concentrations.散射比浊法当混悬液在垂直于入射光的方向察看，因混悬液粒子产生的反射，系统出现乳光(丁达尔效应).。进入一个污浊液的光束，一部分被透过，一部分被吸收，节余部分被悬浊粒子散射。如果在与光束90°的方向检测，若是粒子数量和大小对散射的影响维持常数，能够用悬浊粒子的光散射来测定他们的浓度。照溶液的浊度必须保持不变，并且样品和比较混悬液在同样的条件下制备。丁达尔效应)依靠于粒子的大小和数量。在低浊度范围，光散射浊度法更可靠，散射法浊度单位值和有关检测器信号成线性。随浊浊度的增加，不是所有的粒子都能暴露在入射光下的，并且在抵达检测器的途径中，其他粒子的散射光被阻挡。一个可靠的测量所能测量的最大散射浊度值是1750-2000NTU。必须用起码4个浓度建立标准曲线来证明线性。TurbidimetryTheopticalpropertyexpressedasturbidityistheinteractionbetweenlightandsuspendedparticlesinliquid.Thisisanexpressionoftheopticalpropertythatcauseslighttobescatteredandabsorbedratherthantransmittedinastraightlinethroughthesample.Thequantityofsolidmaterialinsuspensioncanbedeterminedbythemeasurementofthetransmittedlight.Alinearrelationshipbetweenturbidityandconcentrationisobtainedwhentheparticlesizesareuniformandhomogeneousinthesuspension.Thisistrueonlyinverydilutesuspensionscontainingsmallparticles.Linearitybetweenturbidityandconcentrationmustbeestablishedbyconstructingacalibrationcurveusingatleast4concentrations.透射浊度法在液体中悬浊粒子和光之间存在有关性，这一光学特性表示为浊度。表示的是光在直线方向上发生的散射和吸收，而不是光直线经过样品的透射光学特性，经过测量透射光来测定混悬液中固体物质的量。当混悬液中粒子的大小均一且性质相同，可获得浊度和浓度之间的线性关系。只是在很稀的含有少量粒子的混悬液中，才可实现线性。必须使用起码4个浓度建立标准曲线来证明浊度和浓度间呈线性。RatioTurbidimetryInratioturbidimetrytherelationshipofthetransmissionmeasurementtothe90scattered°lightmeasurementisdetermined.Thisprocedurecompensatesforthelightthatisdiminishedbythecolourofthesample.Theinfluenceofthecolourofthesamplemayalsobeeliminatedbyusinganinfraredlight-emittingdiode(IRLED)at860nmasthelightsourceoftheinstrument.Theinstrument’photodiodesdetectorsreceiveandmeasurescatteredlightata90angle°fromthesampleaswellasmeasuringtheforwardscatter(lightreflected)infrontofthesamplealongwiththemeasurementoflighttransmitteddirectlythroughthesample.ThemeasuringresultsaregiveninNTU(ratio)andareobtainedbycalculatingtheratioofthe90anglescattered°lightmeasuredtothesumofthecomponentsofforwardscatteredandtransmittedlightvalues.Inratioturbidimetrytheinfluenceofstraylightbecomesnegligible.Nephelometersareusedformeasurementsofthedegreeofopalescenceofcolourlessliquids.比率透射比浊法测定的是透视光的测量和90°方向上散射光的测量之间的关系。这样的操作补偿了因样品颜色惹起的光衰减。由样品颜色产生的影响也能够用红外发光二级管进行消除，在860nm处的光作为仪器光源。仪器的光电二级管检测器能够获得并测量在样品90°角方向上的散射光。就像测量朝前的散射光（反射光）同样，即当光直接沿浊被测样品经过，被测样品前方的散射光。测量结果以NTU(比率)给出，并经过计算在90°方向上测得的散射光，和向前的散射光和透射光值之和的比率而获得。在比率透射比浊法中，杂散光的影响变得微乎其微。比浊计用于无色溶液乳光度的测量。MeasurementsofreferencesuspensionsI-IVwitharatioturbidimetershowalinearrelationshipbetweentheconcentrationsandmeasuredNTUvalues(seeTable2.2.1.-2).ReferencesuspensionsI-IV(Ph.Eur.)maybeusedascalibratorsfortheinstrument.用比率浊度计对参比悬浊液I-IV的测量，显示了浓度和测量的NTU值之间的线性关系。参比混悬液I-IV(Ph.Eur.)能够用来校正仪器。FormazinsuspensionsOpalescentvalues(NTU)福尔马肼悬浮液乳光值（NTU）ReferencesuspensionI参比悬浊液I3ReferencesuspensionII参比悬浊液II6ReferencesuspensionIII参比悬浊液III18ReferencesuspensionIV参比悬浊液IV30Standardofopalescence乳光标准60Primaryopalescentsuspension4000乳光悬浊液储备液INSTRUMENTALDETERMINATIONOFOPALESCENCE乳光的仪器测定Requirementsinmonographsareexpressedintermsofthevisualexaminationmethodwiththedefinedreferencesuspensions.InstrumentalmethodsmayalsobeusedfordeterminingcompliancewithmonographrequirementsoncethesuitabilityoftheinstrumentasdescribedbelowhasbeenestablishedandcalibrationwithreferencesuspensionsI-IVandwithwaterRorthesolventusedhasbeenperformed.乳光的仪器测定在用正确的参比混悬液定义可见方法时已表示了要求。一旦后边所规定的成立了仪器的适应性，并用参比混悬液I-IV和水或使用的溶剂进行校正，文中的方法也使用于仪器校正。Apparatus.Ratioturbidimetersornephelometerswithselectableratioapplicationuseaslightsourceatungstenlampwithspectralsensitivityatabout550nmoperatingatafilamentcolourtemperatureof2700K,orIRLEDhavinganemissionmaximumat860nmwitha60nmspectralbandwidth.Othersuitablelightsourcesmayalsobeused.Siliconphotodiodesandphotomultipliersarecommonlyusedasdetectorsandrecordchangesinlightscatteredortransmittedbythesample.Thelightscatteredat902.5°isdetected±bytheprimarydetector.Otherdetectorsarethosetodetectbackandforwardscatteraswellastransmittedlight.Theinstrumentsusedarecalibratedagainststandardsofknownturbidityandarecapableofautomaticdeterminationofturbidity.ThetestresultsexpressedinNTUunitsareobtaineddirectlyfromtheinstrumentandcomparedtothespecificationsintheindividualmonographs.仪器：使用可选择的比率浊度计和浊度计时，用钨灯作光源，在2700K的谱线标记温度时，钨灯在大概550nm处有特殊选择性，或许用在860nm处有最大发射并且有60nm光谱宽度的红外发光二级管。也能够使用其他合适的光源。常用硅制光电二极管和光电倍增管作检测器，并记录因样品产生的光散射或光透射的改变。主要检测器检测在90±2.5°方向上的光散射。其他的检测器检测朝后和朝前的光散射，就像测光透射同样。使用的仪器用已知浊度的标准溶液来校正，并能够自动测定浊度。从仪器上直接获得用NTU单位表示的测定结果，并且，在个别文中与规定进行比较。Instrumentscomplyingwiththefollowingspecificationsaresuitable.根据后边的 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使用仪器—Measuringunits:NTU.NTUisbasedontheturbidityofaprimaryreferencestandardofformazin.FTU(FormazinTurbidityUnits)orFNU(FormazinNephelometryUnits)arealsoused,andareequivalenttoNTUinlowregions(upto40NTU).Theseunitsareusedinall3instrumentalmethods(nephelometry,turbidimetryandratioturbidimetry).—测量单位：NTU，NTU根据的是福尔马肼标准储备液的浊度。液使用FTU（福尔马肼浊度单位）或FNU（福尔马肼散射测浊法单位）单位，在低浊度范围内等于NTU（大于40NTU）。这些单位在散射测浊法、浊度法、比率浊度法，三种仪器方法中均可使用。—Measuringrange:0.01-1100NTU.—测量范围：0.01-1100NTU—Resolution:0.01NTUwithintherangeof0-10NTU,0.1NTUwithintherangeof10-100NTU,and1NTUfortherange>100NTU.Theinstrumentiscalibratedandcontrolledwithreferencestandardsofformazin.—分辨率：在0-10NTU范围内分辨率为0.01NTU，在10-100NTU范围内分辨率为0.1NTU，在>100NTU范围内分辨率为1NTU。用福尔马肼的参比标准校正和控制仪器。—Accuracy:0-10NTU:±(2percentofreading+0.01)NTU.10-1000NTU:5per±cent.—精准度：0-10NTU±（2%测量读数+0.01）NTU，10-1000NTU:±5%—Repeatability:0-10NTU:0±.01NTU.10-1000NTU:±2percentofthemeasuredvalue.—重复性：0-10NTU±0.01NTU，10-1000NTU±2%的测量值—Calibration:with4referencesuspensionsofformazinintherangeofinterest.Referencesuspensionsdescribedinthischapterorsuitablereferencestandardscalibratedagainsttheprimaryreferencesuspensionsmaybeused.—校正：用在感兴趣范围内的4中福尔马肼参比混悬液。能够用按本章规定的参比混悬液或合适的相对于参比混悬液储备液标有刻度的参比标准来校正。—Straylight:thisisasignificantsourceoferrorinlowlevelturbidimetricmeasurement;straylightreachesthedetectorofanopticalsystem,butdoesnotcomefromthesample;<0.15NTUfortherange0-10NTU,<0.5NTUfortherange10-1000NTU.—杂散光：在低水平的浊度测定中，杂散光是主要的误差根源。杂散光就是能抵达光学系统的检测器，但不是由于样品而产生的光。0-10NTU的范围内杂散光<0.15NTU，10-100NTU的范围内杂散光<0.5NTU。InstrumentscomplyingwiththeabovecharacteristicsandverifiedusingthereferencesuspensionsdescribedunderVisualmethodmaybeusedinsteadofvisualexaminationfordeterminationofcompliancewithmonographrequirements.切合上面的特性，并用在可见方法下规定的参比混悬液进行校正的仪器，仪器可替代可视检查，这些检查和文中要求一致。在这范围内，这些Instrumentswithrangeorresolution,accuracyandrepeatabilitycapabilitiesotherthanthosementionedabovemaybeusedprovidedtheyaresufficientlyvalidatedandarecapablefortheintendeduse.Thetestmethodologyforthespecificsubstance/producttobeanalysedmustalsobevalidatedtodemonstrateitsanalyticalcapability.Theinstrumentandmethodologyshouldbeconsistentwiththeattributesoftheproducttobetested.所提供的仪器的使用范围、分辨率、正确度、重复性、容量及其余上面提到的参数，这些是十分有效的并能够预期使用。对于剖析特殊的物质/产品，也必须进行试验方法学考证来说明其剖析能力。仪器和方法学应当和测试样品的特性一致。