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机构地区:[1]中山大学药学院,广州510006
出 处:《中国药师》2018年第1期75-78,共4页China Pharmacist
基 金:广东省科技厅产学研项目(编号:2013B090600058;2013B090500100)
摘 要:目的:建立分子蒸馏技术纯化荜澄茄挥发油中柠檬醛的方法。方法:以市售荜澄茄挥发油为原料,采用两次分子蒸馏纯化柠檬醛,主要考察温度对一、二次分子蒸馏纯化效果的影响,所得样品经气相色谱(GC)法分析,通过面积归一化法评价纯化效果。第一次分子蒸馏条件为真空度:3 000 Pa,刮膜转数:300 r·min^(-1),进料流速:7.5 ml·min^(-1),冷却温度:5℃,蒸馏温度:45℃;第二次分子蒸馏条件为真空度:5 Pa,刮膜转速:300 r·min^(-1),进料流速:7.5ml·min^(-1),蒸馏温度:45℃;GC条件为进样量1μl;柱温由70℃程序升温至250℃;分流比1∶100,载气流速1.0 ml·min^(-1)。结果:得到的柠檬醛含量达95.0%,得率为87.5%。结论:建立了两次分子蒸馏结合气相色谱纯化检测荜澄茄挥发油中柠檬醛的方法,为进一步研究荜澄茄成分及柠檬醛的制备提供参考。Objective: To establish the purification process of citral in volatile oil from Fructus Litseae by molecular distillation. Methods: The twice molecular distillation, GC and area normalization method were used for extracting citral, detecting the contents and describing the efficacy of purification, respectively. The mainly factor concerned was temperature. The conditions were as follows: the system pressure was 3 000 Pa, the scraper speed was 300 r min-1 , the feeding rate was 7.5 ml min-1 and the distillation tem- perature was 45 ℃ for the first time molecular distillation; the system pressure was 5 Pa, the scraper speed was 300 r min-1, the feeding rate was 7.5 ml min-t and the distillation temperature was 45 ℃ for the second time molecular distillation. GC was utilized under the following conditions : the sample injection was 1 μl, the column temperature was programmed from 70℃to 250℃, the split ratio was 1:100 and the flow rate of carrier gas was 1.0 ml min-1. Results: The content and yield of citral was up to 95.0% and 87.5%, respectively. Conclusion: The method of twice molecular distillation in combination with GC to purify and detect citral is es- tablished in the work, which can provide reference for the research on the chemical components of Litsea cubeba( Lour. ) Pets. and the preparation of citral.
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