中药化学实用技术Practical technique of Chinese Medicine Chemistry.docx
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中药化学实用技术Practical technique of Chinese Medicine Chemistry.docx
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中药化学实用技术PracticaltechniqueofChineseMedicineChemistry
中药化学实用技术(PracticaltechniqueofChineseMedicineChemistry)
PracticaltechnologyofChineseMedicineChemistry
The|applicationmaterials|coursewareandlessonplans|studyguide||teachingvideosimulationtrainingexercises||caseexamination|evidencematerials|interactiveteaching
Atrainingproject
Twotrainingproject
Threetrainingproject
Fourtrainingproject
Fivetrainingproject
Sixtrainingproject
Seventrainingproject
Eighttrainingproject
Ninetrainingproject
Tentrainingproject
Eleventrainingproject
Doestrainingguide
"Chinesechemicaltrainingpracticaltechnicalguidance"
Isolationandidentificationoffreeanthraquinonesinrhubarbfivetrainingproject
[Objective]training
The1.iscapableofusingrefluxextractionmethodtoextracttotalanthraquinonesinRhubarb
2.proficientinpHgradientextractionoffreeanthraquinonesinrhubarbwereisolated.
3.correctjudgmentofcolorreactionandTLCresults
[training]principle
Rhubarbcontainsemodinanthraquinoneglycosides,theuseoftrainingofanthraquinonesinRhubarbcanbesolubleinethanolandextraction,accordingtothesolubilityoffreeanthraquinonesandanthraquinoneglycosidesinwaterandetherindifferentextractionseparationmethod.Theseparationoffreeanthraquinoneistheuseofanthraquinonesindifferentacidic,usingpHgradientextraction.
[materials]training
RoundbottomflaskcondensingtubemortarbathseparatoryfunnelbeakerflaskdishtubechromatographycylinderpHdipstickTLCsilicagelCMC-Narhubarbpowder
95%5%KOH5%Na2CO35%NaHCO3chloroformetherandethanolhydrochloride0.5%NaOH
Xinhuafilterpaperchromatography(20cm*7cm)-benzeneethylacetate(8:
2)benzenemethanol(8:
1)tolueneammonia0.5%magnesiumacetate1%Rheinchloroformsolution
1%emodinsolution1%aloeemodinchloroformsolution
[training]steps
Total1.ethanolextractpreparation
Extractionofanthraquinones
Takecruderhubarbpowder50g,500mlintheroundbottomflask,add95%ethanoltothehigherdegreeofpowderwasborn,thewaterbathheatingrefluxfor2to3hours,whilehotfiltration.Theresiduewith95%ethanolandthenheatfortwotimes,whilethethreeethanolextractwithhotfiltration.Theconcentratedextractofethanol,ethanolextractobtained.
2.extractionofTotalAnthraquinone,lipophilicandhydrophilicconstituents
Thetotalamountofwaterethanolextractsuspension,add150mlofetherat500mlextractionfunnel,fulloscillationaftertheplacement,pourouttheetherlayer,add50mlofethershake,placed,pourouttheetherlayer,withthemethodoftheoperation6times,untiltheliquidethercolorisshallow,withetherliquidtheethersolutioncontainingtotalanthraquinone.
3.anthraquinonemonomerseparation
SeparationofRhein
Separatoryfunnelto250mlethersolutioncontainingfreeanthraquinoneinaqueoussolutionwith5%NaHCO320ml,shaking.Placethestratification,releasedlowerNaHCO3solution,inanothertriangleflask,theethersolutionretainedinaseparatoryfunnel,
Add5%NaHCO315mlsolutionextractiontime,everytimeaftertheshakingextraction,placedlayeredtimeshouldbeslightlylonger,soastoavoidtheethersolutionmixedinlowerwatersolution,affecttheseparationeffect.Intheprocessofextraction,suchasethercanbeaddedvolatile.WithNaHCO3extract,payattentiontothecolor,carefullyaddinghydrochloricacidtoadjustpH2~3understirring,observetheacidificationprocessofcolorchange,theprecipitateswerecollectedandweighedafterdrying.
Theseparationofemodin
Remaininaseparatoryfunnelethersolution,with5%Na2CO3solutionevery15~20mlabovethesameextractionmethodseveraltimesuntiltheextractcolorisshallow,about6~7times,withNa2CO3extract,carefullyaddinghydrochloricacidtopH2~3,tobeplacedinprecipitation,werecollectedbyprecipitationwaterwashing,drytothesurfaceplate,afterdryingandweighing.
TheseparationofAloeEmodin
Remainliquidseparatingfunnelether,0.5%NaOHaqueoussolutionby15mlextractionof3~4timeseverytime.Theethersolutionwithdistilledwaterextractionof2~3times,towashawaythelye.ExtractwithNaOHandwater,addinghydrochloricacidtoadjustthepH2~3placement.Filtrationprecipitation,precipitationwascollected,washed,driedtothesurfaceplate,afterdryingandweighing.
Theseparationofchrysophanolandemodin-6-ether
Etherliquidretention,recoveryoftheetherroundbottomflask,placed.Werecollectedbywashing,precipitation,drytothesurfaceplate,afterdryingandweighing.
4..
(1)testweretaken:
alkalicrystallizationofanthraquinonecompoundsatesttube,add1mlethanolsolution,addenddropsof5%potassiumhydroxidesolutionwasredreagentshake.
(2):
takethetestofmagnesiumacetatecrystallizationofanthraquinonecompoundsatesttube,add1mlethanolsolution,addenddropsof0.5%magnesiumacetatereagent,produceorange,red,purpleandothercolors.
(3)TLCidentification
Adsorbents:
silicagelCMC-Naplate.
Sample:
1%differentanthraquinonecomponentsinchloroformsolution
Reference:
1%Rheinemodinchloroformsolution;1%chloroformsolution;1%aloeemodinchloroformsolution
Agent:
benzene-ethylacetate(8:
2);benzenemethanol(8:
1)
Color:
Observationofammoniawasobservedafterspraying5%potassiumhydroxidesolution
(4)thepaperchromatographydetection
Supportagent:
Xinhuafilterpaperchromatography(mediumand20cm*7cm)
All1%samples:
Anthraquinonechloroformsolution
Reference:
1%Rheinemodinchloroformsolution;1%chloroformsolution;1%aloeemodinchloroformsolution
Solvent:
toluene
Chromogenicagent:
0.5%magnesiumacetatemethanolsolution
[training]thinking
1.inthetrainingprocessusingthepHgradientextractionseparationoffreeanthraquinoneextractionprocessiftheemulsificationphenomenon,shouldbehowtodealwith?
2.chrysophanolandphyscioninsimilarstructure,pleasedesignseparationmethod.
Shouldpayattentiontowhatthe3.safetyproblemsinthetraining?
Reportextractionandidentificationoffreeanthraquinonesinrhubarbtraining
Theclassnameofschooltrainingtime
1.trainingobjective
2.telltheextractionprincipleoffreeanthraquinonesinRhubarb
3.procedures:
(1)anthraquinoneextractionandseparationprocessofrhubarb
(2)thinlayerchromatographyandpaperchromatographyprocess
4.trainingrecords
Theextractionresultsrecorded
Theextractionrateofextractextractweight(%).
Rhein(g)
Emodin(g)
Aloeemodin(g)
Chrysophanolandphyscion(g)
Resultstestrecord
Theconclusionandinterpretationofthephenomenonofthesample
Alkalimagnesiumacetatetesttest
Rhein
Emodin
AloeEmodin
Chrysophanolandphyscion
RecordsoftheresultsofTLC
Thestandardsolutionofsamplesolution
Rheinandemodinaloeemodinrheinandemodinandaloeemodin
Spotcolor
Theorigintothespotcenterdistance(CM)
Thedistancefromtheorigintotheedgeofthesolvent(CM)
Rf
Schematicdiagramoftlc:
Recordsoftheresultsofpaperchromatography
Thestandardsolutionofsamplesolution
Rheinandemodinaloeemodinrheinandemodinandaloeemodin
Spotcolor
Theorigintothespotcenterdistance(CM)
Thedistancefromtheorigintotheedgeofthesolvent(CM)
Rf
Schematicdiagramofpaperchromatography:
5.trainingsummaryanddiscussion
6.thinkingtraining
7.teachercomments
Teachersignaturedate
IsolationandidentificationoftrainingtestoffreeanthraquinonesinRhubarb
Projectskilltestingstandardscorescoreremarks
call
1,choosetherightbalanceplacedsmoothly2
2,eachweighingbeforeadjustingthe"0"2
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