高纯度天然右旋龙脑的制备研究_宋永芳

SONGYF宋永芳,罗嘉梁(中国林业科学研究院林产化学工业研究所,江苏南京210042)　:　[Cinnamomumglanduliferum(Wall)Nees]、70%～80%d-。d-,、、d-。GC、GC/MSd-,d-。,d-,1∶1.7～2.0、4d,d-99%。d-:,99%,[α]20D+37°,205～209℃,5×10-6,(As)2×10-6。:　;d-;;:S792.23;R282.71　　　　:A　　　　:0253-2417(2003)03-0011-04STUDYONPREPARATIONOFHIGH-PURITYNATURALd-BORNEOLSONGYong-fang,LUOJia-liang(InstituteofChemicalIndustryofForestProducts,CAF,Nanjing210042,China)Abstract:Cruded-borneolwasobtainedbywatervapordistillationandsublimationfromleavesofCinnamomumglanduliferum(Wall)Nees.Inordertopreparehigh-purityd-borneol,experimentswerecarriedouttoinvestigatetheeffectsofdifferentsolvent,solventamount,timesofcrystallizationandcrystallizingtime.High-purityd-borneolwasanalyzedbyGCandGC/MS,andcrystalofd-borneolwasexaminedbyscanningelectronmicroscopy(SEM).Resultsshowedthatgasolineisthebestsolventforcrystallizingd-borneol,purityofd-borneolproductwasover99%usingmaterial:solventratio1∶1.7-2.0,andcrystallizingtime4days.Analyticaldataofthefinenaturald-bor-neolproductsare:appearanceofwhiteslicecrystals,d-borneolcontent99%,opticalrotation[α]20d+37,meltingpoint205-209℃,heavymetalscontent5millionthandarsenide(As)content2millionth.Keywords:Cinnamomumglanduliferum(Wall)Nees;naturald-borneol;SEM;crystallization,[1]《》,。,。、、、、、,、、、、。,、,。:2002-10-11　:1996(96-10)　:(1940-),,,,。23320039　　　　　　ChemistryandIndustryofForestProductsVol.23No.3Sept.2003,,(),()(、)。,2000～20011000t/a。,500～600t/a,,200t,300t。,[2]、、,,、,。,,。,d-,GC、GC/MSd-,d-。1　1.1　、。Cinnamomumglanduliferum(Wall.)Nees,。1.2　1.3　d-GC-7AG,:DB-5(30m×0.32mm);200℃;100℃;1/50,0.1μL。1.4　d-,。1.5　d-:JMS-D300GC/MScomp;:SE30(30m×0.25mm);:230℃;130℃(2min)5℃/min160℃;EI,70eV,3kV;300μA,190℃,2s;(m/z)35～250,GC/MS;GC/MS:180℃。1.6　d-LBS5SEM-505。2　2.1　,d-。1　Table1　SelectionoffinetreefromcamphortreesNo.d-/%d-borneolcontent[α]20Dopticalrotation/%camphor/%low-boiler181.2+32.49.509.3272.3+31.420.607.0471.6+31.022.07.152.6+34.282.5014.9681.9+35.217.320.7786.1+36.413.89—2.1.1　富含d-龙脑优株樟树的筛选　1。1,7d-,,61。,。5,。2.1.2　不同季节樟树叶中含d-龙脑比较　1997～1998,。。2。12　　　　　　　　　232　d-Table2　d-Borneolcontentoftwigsandleavesindifferentseasonsdate/gtwigsandleaves/%moisturecontentd-/gd-borneol/%yieldd-/%d-borneolcontent1997-04-2360010.386.01.1185.301997-04-2364410.837.51.2985.411997-07-2245015.967.01.8586.531997-07-2244515.967.01.8787.511997-10-22150053.011.81.6786.261997-10-22100048.08.81.6986.101998-01-3055050.012.02.1881.591998-01-3055050.012.52.2081.64　　d-,,。1。2.2　,。,。Sigma,85%d-100g39.0,98%(GC)d-250mg13.9,,。。2.2.1　结晶次数与d-龙脑含量影响　,,,3。3　d-Table3　d-Borneolcontentincrystallizingprocess/gdosagefirstcrystallizingmass/gcontent/%secondarycrystallizingmass/gcontent/%thirdcrystallizingmass/gcontent/%30014393.264570.001860.1030014292.804671.301858.92　　3,80%d-92%,,。2.2.2　溶剂比对d-龙脑结晶质量的影响　,,,,,,,4。4　d-Table4　Effectofsolventamountond-borneolcrystallizingNo./g∶/mLmaterial∶solventcrystallizingsituationd-/%d-borneolcontent191∶1.20powder89.32201∶1.50granular92.94211∶1.66piece93.26221∶1.74slice95.50231∶1.92bigslice97.15241∶2.15bigslice97.505　d-Table5　Effectsofcrystallizingtimeond-broneolqualitytimeappearances/%content6hpowder83.124h　granular88.04dslice95.55dslice96.66dbigslice97.54,,,,1∶1.7～2.0,95%。1　d-GCFig.1　GCspectrumoffined-borneol2.2.3　结晶时间对d-龙脑品质的影响　100g(81%),,,。,4d95%,,,5。2.2.4　高纯度d-龙脑的制备　,、、d-99%(GC),[α]20D+37(C2H5OH)。GC/MS,(98)()(20554)。。(95)()(V0236),1、2。3,:13　　　2　d-Fig.2　MSspectrumoffined-borneol2.2.5　精制d-龙脑有关质量指标分析　d-,,[3]。d-:,99%,[α]20D+37°,205～209℃,5×10-6,(As)2×10-6。2.2.6　d-龙脑晶体的电子显微镜观察　,。GC,3　d-Fig.3　SEMphotographofd-borneolA.d-d-borneolbyalcoholcrystallizing(95%);B.d-d-borneolbypetroleumethercrystallizing(90%);C.d-cruded-borneol(80%);D.d-fined-borneol(99%);E.syntheticborneol(52%)。[4],d-。d-,d-,。3。3,d-(A);d-(B);d-,,(C);99%d-,(D);,(E)。d-。3　3.1　d-,d-1.11%～2.20%,80%。,d-。,,1。3.2　,∶1∶1.7～2.0,4d,95%。、d-99%。3.3　d-,d-,。:[1].()[M].:,1982.:1965-1968.[2],.[J].,1990,25(1):19-22.[3].,[M].:,2000.:113-114.[4],.[J].,1994,25(5):241-244.14　　　　　　　　　23