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机构地区:[1]中国林业科学研究院林产化学工业研究所,江苏南京210042
出 处:《林产化学与工业》2003年第3期11-14,共4页Chemistry and Industry of Forest Products
基 金:原林业部1996年重点项目(96 10)
摘 要: 以樟树[Cinnamomumglanduliferum(Wall)Nees]枝叶为原料经水蒸气蒸馏、升华得到70%~80%粗d 龙脑。为制备高纯度天然d 龙脑,进行了不同溶剂、不同溶剂量、结晶次数和结晶时间对d 龙脑纯度影响的研究。并用GC、GC/MS分析鉴定所制备的天然d 龙脑,用扫描电子显微镜观察d 龙脑结晶过程中晶体的结构变化。结果表明,汽油是结晶d 龙脑最好的溶剂,当物料比为1∶1.7~2.0、结晶时间4d以上时,天然d 龙脑的纯度可达99%以上。精制天然d 龙脑产品的分析数据为:外观白色片状结晶,右旋龙脑含量>99%,旋光度[α]20D>+37°,熔点205~209℃,重金属<5×10-6,砷(As)<2×10-6。Crude dborneol was obtained by water vapor distillation and sublimation from leaves of Cinnamomum glanduliferum(Wall) Nees.In order to prepare highpurity dborneol,experiments were carried out to investigate the effects of different solvent,solvent amount, times of crystallization and crystallizing time.Highpurity dborneol was analyzed by GC and GC/MS,and crystal of dborneol was examined by scanning electron microscopy(SEM).Results showed that gasoline is the best solvent for crystallizing dborneol,purity of dborneol product was over 99% using material:solvent ratio 1∶1.7-2.0,and crystallizing time 4 days.Analytical data of the fine natural dborneol products are:appearance of white slice crystals,dborneol content>99%,optical rotation \20d>+37,melting point 205-209 ℃,heavy metals content <5 millionth and arsenide(As) content<2 millionth.
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