文档介绍:该【LC-MS液质联用资料系列 】是由【相惜】上传分享,文档一共【35】页,该文档可以免费在线阅读,需要了解更多关于【LC-MS液质联用资料系列 】的内容,可以使用淘豆网的站内搜索功能,选择自己适合的文档,以下文字是截取该文章内的部分文字,如需要获得完整电子版,请下载此文档到您的设备,方便您编辑和打印。Massspectrometryforthechromatographer整理ppt??????LC/MSinDrugDevelopmentIdentifyunknownpeakstosupportmethoddevelopmentandvalidationCharacterizedegradationproductsinforceddegradationstudiesandstabilitysamplesElucidatedrugdegradationpathwaytosupportexcipientselectionandformulationdevelopmentConfirmpeakidentityforDSandrelatedsubstancesSupportQAissuesandNDASupportManufacturingprocessandfinisheddrugproducts整理pptFeaturesofLC/MSAdvantages:?Highsensitivity?Highselectivity?Speed?Combinedpowerofseparationandidentification?MolecularweightandstructureinformationDisadvantages:?poundsarenotionizable?pleteunknowns?paredtoNMR整理pptIdentificationStrategy:WhenyoustartLC/MSanalysis…..?patible??poundsform?Syntheticscheme(Byproduct?Intermediate?)?StructureofdrugsubstanceactivesitesandfunctionalgroupsNumberofnitrogenatoms,Isotoperatio?FullMSspectrumofunknown:Whichis[M+H]??MS/MSspectraofDSandunknown?UVspectraofDSandunknown整理pptLC/MSAnalysis WorkRequestLC/patiblemethod ConfirmChromatogramSelectIonizationModeESIvsAPCI,(+)vs(-)LC/patiblemethod onditions ShowPeakEquivalencyDetermineMWMS/MS(n)StudyIsolation/PurificationProposedStructure NMRConfirmationReportNoConfirmation?YesIn-houseSynthesis整理pptLC-MSLCInterfaceExtractionof –SeparationofthemixtureofanalytesInterface–SeparationoftheanalytefromthesolventMA(massanalyzer)–separationoftheanalytemolecularordingtotheirmasstochargeratio整理pptInfusionMSMicroTeeMSLC100μl/minpump 1μl/min Samplesolution ?Sampleincontinuousflow ?Nosampleinjection ?NoLCseparation ?MSspectrumobtainedoverangiventime ?ImprovedS/Nduetotheaverageofmultiplespectra ?SelectLCflowtoassistionization整理ppt-4BasicElectrospraySchematic N760Torr1Torr10-2–10-5Torr10-5TorrIonoptics ,ElectrosprayIonizationMassSpectrometry,FundamentalsInstrumentationandApplications,WileyInterscience,1997整理ppt??????ELECTROSPRAYFactorstoconsiderIonicstrengthSurfacetensionofthesolventVolatilityofthesolventCharacteroftheanalyteionsinsolution:solvated,ionpaired,etcpositionandamountofwaterpHofthemobilephase整理pptIntensityIntensityConfirmationofmolecularweightESI(+)ESI(-)