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volatile oilEssentialoil(volatileoil)ⅡTheconstitutionofessentialoils1.terpenoidsmonoterpenoids,sesquiterpenoidsandtheiroxygen-containingderivatives.mentholcitral2.aromaticcompoundscinnamaldehydexanthoxylin3.aliphaticcompoundsCH3-(CH2)7-CH2OH正壬醇4.othercompoundsCH2=CH-CH2-N...

volatile oil
Essentialoil(volatileoil)ⅡTheconstitutionofessentialoils1.terpenoidsmonoterpenoids,sesquiterpenoidsandtheiroxygen-containingderivatives.mentholcitral2.aromaticcompoundscinnamaldehydexanthoxylin3.aliphaticcompoundsCH3-(CH2)7-CH2OH正壬醇4.othercompoundsCH2=CH-CH2-N=C=S异硫氰酸烯丙酯Ⅲproperties1.Descriptioncolorlessoryellowishtransparentliquidatroomtemperature,strongspecificodour.2.volatilityvolatileatroomtemperature,notrace.3.solubilityessentialoilcan’tdissolveinH2O,easilydissolveinorganicsolvent,p.e.,Et2O,CS2,candissolveinhighconcentrationEtOHcompletely,dissolveinlowconcentrationEtOHpartly.4.physicalconstantrelativedensity:0.85-1.065opticalactivity:specificrotation(比旋度):+97°~117°.Refractiveindex(折光率):1.43~1.61Boilingpoint:70℃~300℃.5.stabilitycontactingwithairorlightleadtooxidationanddegeneracy,sothevolatileoilsshouldbestoredinbrownbottleairtightlyandinlowtemperature.ⅣExtractionandisolation1.Extraction1.1steamdistillation1.2extractionwithsolventsorganicsolventswithlowboilingpoint,toomuchlipophillicimpurities.1.3absorptionexpensiveoil.1.4extractionbycrushing1.5SFE-CO22.Isolation2.1freezing薄荷油析出粗脑油析出粗脑较纯薄荷脑-10℃放置12小时(第一批)(第二批)-20℃冷冻24小时加热熔融0℃冷冻Therulesofboilingpoint:1.Thenumberofcarbonatom:themore→thehigher2.Thenumberofdoublebond:themore→thehigher3.Thenumberofoxygenatom:themore→thehigher4.functionalgroup:themorepolar→thehigher-COOH>R-OH>R-CO-R~R-CHO>R-O-R2.2fractionating2.3chemicalmethod(1)basiccompounds:extractwith1%H2SO4orHCl(2)acidcompounds:extractwithNaHCO3,NaOH(3)R-OH(4)CompoundswithC=O:NaHSO3orGirardreagents挥发油/Et2O水洗,5%NaHCO3萃取酸水层乙醚层10%HCl萃取碱性成分碱水层乙醚层碱化;醚萃挥发性Alk酸化;醚萃强酸性成分萜酸、挥发性酸1~2%NaOH萃取四、挥发油成分的分离㈢化学方法碱水层乙醚层酸化;醚萃1~2%NaOH萃取碱水层乙醚层酸化;醚萃醛酮等羰基化合物乙醚层弱酸性成分酚、烯醇、内酯1.邻苯二甲酸酐2.碱液萃取30%NaHSO3萃取含中性成分四、挥发油成分的分离㈢化学方法乙醚层1.邻苯二甲酸酐2.碱液萃取碱水层乙醚层分馏或柱色谱皂化,醚萃萜醇ⅠⅡⅢ……(terpenoidacidandvolatileacid)Essentialoil/Et2OExtractwith1%-2%HClH+/H2OEt2Oalkalify,extractwithEt2Oextractwith5%NaHCO3Et2OOH-/H2OEt2OAcidify,ExtractwithEt2Oextractwith1%-2%NaOHEt2OEt2OOH-/H2OAdd30-40%NaHSO3orGirardreagentsacidify,ExtractwithEt2OEt2O(basiccompounds)(additionproduction)(compoundwithcarbonyl)(terpenoidalcohol)PptorH2OsolutionaddNaOHoracidtodecompose,extractwithEt2OEt2OEt2Oesterifywithphthalicanhydride,extractwith5%NaHCO3OillayerOH-/H2OsaponifywithNaOH,extractwithEt2OEt2OⅠⅡⅢ2.4chromatographyAgNO3silicagelorAgNO3Al2O32-25%AgNO3factorsaffectingthecomplex:(1)  thenumbersofdoublebond(2)  cis>trans(3)terminaldoublebond>othersitesα-asaroneβ-asaroneeduasaroneelutingwithbenzene:Et2O(5:1)elutingsequenceα-asarone,β-asarone,eduasaroneⅤidentificationofessentialoil1. Determinationofphysicalconstantsrelativedensity;specificrotation;refractiveindex.2. Determiantionofchemicalconstantsacidvalue;estervalue;saponificationvalue.3. Identificationoffunctionalgroup4. IdentificationbychromatographyTLC;GC;GC-MS.
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