分享天然产物分离 Natural Products Isolation 02

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1、IsolationbyPlanarChromatography231DevelopmentCompoundBandsFig.7.CircularbandseparationthroughCPTLCdevelopment.Me;1MeCompound5.mobilephaseofpetrol/ethylacetate(49:1)wereusedandthecompoundwasvisualizedunderUVlight.WatermanandAmpofo(12)usedCPTLCtoisolatethecytotoxicquassinolds,ailanthinone(

2、Compound6),2’-acetylglaucarubinone(Com-pound7)andthealkaloid8-hydroxycanthin-6-one(Compound8)fromtherainforesttreeOdyendyeagabonensis(Simaroubaceae).6.Over-PressureTLC(OPTLC)Over-pressureTLC(OPTLC)wasintroducedbyTyihaketal.in1979(13)manattempttocombmetheadvantagesofconventionalTLCandHPLC

3、.Thistechniqueemploystheuseofapressurizedcircularultramicrochamber(PUMchamber),whichhousesaTLCplateandinletsfortheintroductionofsampleandsolventontothesorbent.Thethinsorbentlayeriscoveredbyamembranekeptunderexternalpressuresothatthevaporphaseabovethesorbentisnearlyeliminated.Asubstantial

4、lyshortertimeisrequiredforseparationthanincon-ventionalTLCandclassicalcolumnchromatography(CC)andgreaterresolu-tionandseparationefficiencyISachieved.TherateatwhichsolventmigratesISasstableasHPLCandconsequentlythetechniquecanbeusedtomodelCC232GibbonsandGrayOH0YCompound6and7.(6)R=COCH(Me)C

5、H,CH,.(7)R=COC(OAc)(Me)CH,CH,(silicagel;CH,Cl,-lsopropanol[49:11).Compound8.(sdlcagel;toluene:EtOAc’AcOH[5.4.1]).methods.Separationscanbecarriedout5-20timesfasterthanconventionalTLC,andsothismethodmaybeapplicabletohighthroughput/repetitions.Tyihaketal.validatedthistechniqueusingthesepara

6、tionofthesyntheticdyesindophenol,SudanG,andButterYellow.Naturalproductssuchascap-saicinfromCapscumanuumandfurocoumarinsfromHeracleumsphondyliumhavebeenseparatedbyNyirdeyetal.(14).6.1.AutomatedMultipleDevelopment(AMD)Tinsmethodutilizesafullyautomateddevelopmgchamberthatconsistsofasensorto

7、opticallydetectthesolventfrontposition,amechamsmtolifttheplateoutofthedevelopingchamber,multiplesolventreservoirs,asolventpump,andanintegratedfantodrytheplateandremovesolventvapor.Modemsystemscontainmicroprocessor-controlledprogrammingtovarysolventcompositionaftereachrun.