苦参碱和氧化苦参碱的提取分离鉴定ppt.ppt

EXP2 Extraction Isolation andIdentificationofMatrineandOxymatrine EXP1 ThePreparationofThin LayerChromatography TLC SilicaGelPlates 1 Purpose AcquirethepreparationofTLCsilicagelplates 2 PrincipleChromatographyplates 层析板 aglass plastic metalsheetorplateAdsorbents 吸附剂 SilicagelH silicagelG silicagelGF254 silicagelHF254 aluminumoxide polyamideandcelluloseAdhesives 粘合剂 CMC Na PlasterofParis CaSO4 1 2H2O starch 淀粉 Activitygrade fivegradesAdsorption Partition3 ApparatusandReagentsGlassplates5 10 5 or2 5 7 5cm 10 cleananddrysilicaHforTLC0 8 CMC Na EXP1 PreparationofSilicaGelTLCPlates 4 ProceduresforExp 1Itisimportanttoensurethattheglassplatesarecleanandfreegreasebeforeuse Weigh10gsilicaHand30mlCMC Na 0 8 andmixsmoothlyina50mlbeaker Spreadtheslurryquicklyontotheplatesfromonetoanother andthenshaketheplatestoformauniformfilm TransfertheTLCplatestoanevenplaneanddryitintheshade ActivatetheTLCplatesat105oCinanovenfor30minutes AllowtheTLCplatestocooltoroomtemperatureandstoretheminadesiccator EXP1 PreparationofSilicaGelTLCPlates EXP 2 Extraction Isolation andIdentificationofMatrineandOxymatrine 1 PurposeLearnthemethodsofextracting isolatingalkaloidsfromtheplantofSophoraflavescensAit andidentifytheirstructures 2 PrincipleMatrineandoxymatrinefromSophoraflavescensaretertracyclo quinolizindinealkaloids whichcandissolveindiluteacidicsolutiontobecomesalts 2 PrinciplePassthesolutionthroughacolumnofcationexchangeresin H type whichwillabsorbthealkaloids thentheresinwasalkalifiedwithconcentratedNH3 H2OandthealkaloidsmixtureisextractedwithCHCl3 PrincipleofstrongacidiccationexchangeresinRSO3 Na HCl R SO3 H NaClRSO3 H BH Cl RSO3 BH HClRSO3 BH NH3 H2O RSO3 NH4 B H2O EXP 2 Extraction Isolation andIdentificationofMatrineandOxymatrine 3 ApparatusandReagentsAmberliteIRC 50 Constantpressurefunnel etal 4 ProceduresExtractionofmatrineandOxymatrinefromS flavecens 300g 2 2groups crudeslicesofS flavescenswasextractedwith0 5 HCl 3000ml for1dayatroomtemperature Add0 1 sodiumbenzoate 3g Repeattheaboveprocedureonceagain combinethetwiceextract ResinPreparation150gcationexchangeresinwassoakedin2MHClfor45min WashtopH5 7withwater Soaktheresinwith5 NaOHfor45min WashtopH7withwater Soaktheresinwith2MHClfor45min WashtopH7withwater storein500mlbeakerwithwaterandlabelname EXP 2 Extraction Isolation andIdentificationofMatrineandOxymatrine 4 Procedures 3 Exchangeoftheacidicsolutionandprecipitationreactionsofthealkaloids a Theextractionwasfilteredandpassedthroughthepreparedresin flowrate theexchangingendpointwasdetectedbydragendorffreagent WashtheresintopH5 7withwater Thentheresinwasvacuumfilteredandputintoapaperboxforopen airdryingandlabelname EXP 2 Extraction Isolation andIdentificationofMatrineandOxymatrine EXP 2 Extraction Isolation andIdentificationofMatrineandOxymatrine 2020 3 12 9 可编辑 4 Procedures 3 Exchangeoftheacidicsolutionandprecipitationreactionsofthealkaloids b Theplantextractsweretestedforthepresenceofalkaloidswithalkaloid precipitatingreactions Theprecipitationreagentsincludedragendorffreagent碘化铋钾 silicotungsticacid硅钨酸 tannicacid鞣酸 picricacid苦味酸andiodine potassiumiodide 碘 碘化钾 EXP 2 Extraction Isolation andIdentificationofMatrineandOxymatrine EXP 2 Extraction Isolation andIdentificationofMatrineandOxymatrine 来后打开水浴锅开关仪器干燥 包括展开缸 Add20ml 湿润即可 concentratedNH3 H2Ototheresin 4 Procedures 4 Alkalizationoftheresinandextractionofthealkaloids Add20ml 湿润即可 concentratedNH3 H2Ototheresinfor15min transferthemtoaconstantpressurefunnel Extractedwith200mlCHCl3byreflowingfor2hours Theextractionwasdriedwithanhydroussodiumfulfate Na2SO4 for10minandfiltered Thefiltratewasconcentratedbyairdistillation Thevestigialremnantwasadded20mlacetone EXP 2 Extraction Isolation andIdentificationofMatrineandOxymatrine EXP 2 Extraction Isolation andIdentificationofMatrineandOxymatrine 4 Procedures 5 DetectionofMatrineandOxymatrine TLCplates silicagelglassplatesSamples theacetonesolutioncontainingalkaloidsstandardmatrineandoxymatrinesolution 回收 Developingsolvents CHCl3 MeOH 9 1 saturatedwithNH3 H2O Chromogenicagent dragendorffreagentCompareRfvaluesofthesamplewiththatofthestandardm