ASTM F2260-2003(2008) 用质子核磁共振(1HNMR)光谱法测定脱乙酰壳多糖盐的脱乙酰作用程度的标准试验方法
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【英文标准名称】:StandardTestMethodforDeterminingDegreeofDeacetylationinChitosanSaltsbyProtonNuclearMagneticResonance(1HNMR)Spectroscopy
【原文标准名称】:用质子核磁共振(1HNMR)光谱法测定脱乙酰壳多糖盐的脱乙酰作用程度的标准试验方法
【标准号】:ASTMF2260-2003(2008)
【标准状态】:现行
【国别】:美国
【发布日期】:2003
【实施或试行日期】:
【发布单位】:美国材料与试验协会(US-ASTM)
【起草单位】:F04.42
【标准类型】:(TestMethod)
【标准水平】:()
【中文主题词】:
【英文主题词】:Chitosansalts;Deacetylation;GlcNAc;Nuclearmagneticresonance(NMR)spectrometry;TEMPs(tissueengineeredmedicalproducts)
【摘要】:Thedegreeofdeacetylationofchitosansaltsisanimportantcharacterizationparametersincethechargedensityofthechitosanmoleculeisresponsibleforpotentialbiologicalandfunctionaleffects.Thedegreeofdeacetylation(%DA)ofwater-solublechitosansaltscanbedeterminedby1Hnuclearmagneticresonancespectroscopy(1HNMR).SeveralworkershavereportedontheNMRdeterminationofchemicalcompositionandsequentialarrangementofmonomerunitsinchitinandchitosan.ThetestmethoddescribedisprimarilybasedontheworkofV?/span>rumetal.(1991),whichrepresentsthefirstpublicationonroutinedeterminationofchemicalcompositioninchitosansbysolutionstate1HNMRspectroscopy.Thistestmethodisapplicablefordeterminingthe%DAofchitosanchlorideandchitosanglutamatesalts.Itisasimple,rapid,andsuitablemethodforroutineuse.Quantitative1HNMRspectroscopyreportsdirectlyontherelativeconcentrationofchemicallydistinctprotonsinthesample,consequently,noassumptions,calibrationcurvesorcalculationsotherthandeterminationofrelativesignalintensityratiosarenecessary.Inordertoobtainwell-resolvedNMRspectra,depolymerizationofchitosanstoanumberaveragedegreeofpolymerization(DPn)of~15to30isrequired.Thisreducestheviscosityandincreasesthemobilityofthemolecules.Althoughthereareseveraloptionsfordepolymerizationofchitosans,themostconvenientprocedureisthatofnitrousaciddegradationindeuteratedwater.Thereactionisselective,stoichiometricwithrespecttoGlcN,rapid,andeasilycontrolled(Allanx0026;Peyron,1995).ThereactionselectivelycleavesafteraGlcN-residue,transformingitinto2,5-anhydro-D-mannose(chitose),consequently,depletionofGlcNafterdepolymerizationisexpected.Ontheotherhand,thechitoseunitdisplayscharacteristic1HNMRsignalstheintensityofwhichmaybeestimatedandutilizedinthecalculationof%DA,eliminatingtheneedforcorrectionfactors.Usingtheintensityofthechitosesignals,thenumberaveragedegreeofpolymerizationcaneasilybecalculatedasacontrolofthedepolymerization.Samplesareequilibratedandanalyzedatatemperatureof90x00B1;1x00B0;C.Elevatedsampletemperaturecontributestoreducingsampleviscosityandrepositionstheprotonsignalofresidualwatertoanareaoutsidethatofinterest.Whilesamplesarenotstoredat90x00B0;Cbutonlyanalyzedatthiselevatedtemperature,theNMRtubesshouldbesealedwithastoppertoavoidanyevaporation.AtasamplepH*of3.8-4.3(see6.1.5below),artifactualdeacetylationofthesampledoesnotoccurduringtheshortequilibrationandanalysistime.AgeneraldescriptionofNMRcanbefoundinx003C;761>oftheUSP24-NF19.1.1ThistestmethodcoversthedeterminationofthedegreeofdeacetylationinchitosanandchitosansaltsintendedforuseinbiomedicalandpharmaceuticalapplicationsaswellasinTissueEngineeredMedicalProducts(TEMPs)byhigh-resolutionprotonNMR(1HNMR).AguideforthecharacterizationofchitosansaltshasbeenpublishedasGuideF2103.1.2Thetestmethodisapplicablefordeterminingthedegreeofdeacetylation(%DA)ofchitosanchlorideandchitosanglutamatesaltsandisvalidfor%DAvaluesfrom50uptoandincluding99.Itissimple,rapid,andsuitableforroutineuse.KnowledgeofthedegreeofdeacetylationisimportantforanunderstandingofthefunctionalityofchitosansaltsinTEMPformulationsandapplications.Thistestmethodwillassistendusersinchoosing......
【中国标准分类号】:C10
【国际标准分类号】:71_040_50
【页数】:5P.;A4
【正文语种】:英语
【原文标准名称】:用质子核磁共振(1HNMR)光谱法测定脱乙酰壳多糖盐的脱乙酰作用程度的标准试验方法
【标准号】:ASTMF2260-2003(2008)
【标准状态】:现行
【国别】:美国
【发布日期】:2003
【实施或试行日期】:
【发布单位】:美国材料与试验协会(US-ASTM)
【起草单位】:F04.42
【标准类型】:(TestMethod)
【标准水平】:()
【中文主题词】:
【英文主题词】:Chitosansalts;Deacetylation;GlcNAc;Nuclearmagneticresonance(NMR)spectrometry;TEMPs(tissueengineeredmedicalproducts)
【摘要】:Thedegreeofdeacetylationofchitosansaltsisanimportantcharacterizationparametersincethechargedensityofthechitosanmoleculeisresponsibleforpotentialbiologicalandfunctionaleffects.Thedegreeofdeacetylation(%DA)ofwater-solublechitosansaltscanbedeterminedby1Hnuclearmagneticresonancespectroscopy(1HNMR).SeveralworkershavereportedontheNMRdeterminationofchemicalcompositionandsequentialarrangementofmonomerunitsinchitinandchitosan.ThetestmethoddescribedisprimarilybasedontheworkofV?/span>rumetal.(1991),whichrepresentsthefirstpublicationonroutinedeterminationofchemicalcompositioninchitosansbysolutionstate1HNMRspectroscopy.Thistestmethodisapplicablefordeterminingthe%DAofchitosanchlorideandchitosanglutamatesalts.Itisasimple,rapid,andsuitablemethodforroutineuse.Quantitative1HNMRspectroscopyreportsdirectlyontherelativeconcentrationofchemicallydistinctprotonsinthesample,consequently,noassumptions,calibrationcurvesorcalculationsotherthandeterminationofrelativesignalintensityratiosarenecessary.Inordertoobtainwell-resolvedNMRspectra,depolymerizationofchitosanstoanumberaveragedegreeofpolymerization(DPn)of~15to30isrequired.Thisreducestheviscosityandincreasesthemobilityofthemolecules.Althoughthereareseveraloptionsfordepolymerizationofchitosans,themostconvenientprocedureisthatofnitrousaciddegradationindeuteratedwater.Thereactionisselective,stoichiometricwithrespecttoGlcN,rapid,andeasilycontrolled(Allanx0026;Peyron,1995).ThereactionselectivelycleavesafteraGlcN-residue,transformingitinto2,5-anhydro-D-mannose(chitose),consequently,depletionofGlcNafterdepolymerizationisexpected.Ontheotherhand,thechitoseunitdisplayscharacteristic1HNMRsignalstheintensityofwhichmaybeestimatedandutilizedinthecalculationof%DA,eliminatingtheneedforcorrectionfactors.Usingtheintensityofthechitosesignals,thenumberaveragedegreeofpolymerizationcaneasilybecalculatedasacontrolofthedepolymerization.Samplesareequilibratedandanalyzedatatemperatureof90x00B1;1x00B0;C.Elevatedsampletemperaturecontributestoreducingsampleviscosityandrepositionstheprotonsignalofresidualwatertoanareaoutsidethatofinterest.Whilesamplesarenotstoredat90x00B0;Cbutonlyanalyzedatthiselevatedtemperature,theNMRtubesshouldbesealedwithastoppertoavoidanyevaporation.AtasamplepH*of3.8-4.3(see6.1.5below),artifactualdeacetylationofthesampledoesnotoccurduringtheshortequilibrationandanalysistime.AgeneraldescriptionofNMRcanbefoundinx003C;761>oftheUSP24-NF19.1.1ThistestmethodcoversthedeterminationofthedegreeofdeacetylationinchitosanandchitosansaltsintendedforuseinbiomedicalandpharmaceuticalapplicationsaswellasinTissueEngineeredMedicalProducts(TEMPs)byhigh-resolutionprotonNMR(1HNMR).AguideforthecharacterizationofchitosansaltshasbeenpublishedasGuideF2103.1.2Thetestmethodisapplicablefordeterminingthedegreeofdeacetylation(%DA)ofchitosanchlorideandchitosanglutamatesaltsandisvalidfor%DAvaluesfrom50uptoandincluding99.Itissimple,rapid,andsuitableforroutineuse.KnowledgeofthedegreeofdeacetylationisimportantforanunderstandingofthefunctionalityofchitosansaltsinTEMPformulationsandapplications.Thistestmethodwillassistendusersinchoosing......
【中国标准分类号】:C10
【国际标准分类号】:71_040_50
【页数】:5P.;A4
【正文语种】:英语
下载地址: 点击此处下载
