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化学学报
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化学学报 ›› 2001, Vol. 59 ›› Issue (11): 2007-2011. 上一篇    下一篇

研究论文

利用分子识别包结结晶法选择性分离小茴香挥发油中的化学 组分

郭文生;郭放;王秀梅;常怀春;杨春常;唐宪达;葛春华;佟键;王洪波;蔡 云萍;由键;程光荣   

  1. 辽宁大学化学科学与工程学院应用化学研究所;辽宁省分析测试研究中心
  • 发布日期:2001-11-15

Selective isolation of chemical component from volatile oil of xiaohuixiang by molecular cognition inclusion crystalline method

Guo Wensheng;Guo Fang;Wang Xiumei;Chang Huaichun;Yang Chunchang;Tang Xianda;Ge Chunhua;Tong Jian;Wang Hongbo;Cai Yunping;You Jian;Cheng Guangrong   

  • Published:2001-11-15

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646

被引次数

14 | 5

用GC－MS方法测定了小茴香挥发油的全组分，其中对-丙烯基茴香醚的含量为82.65%。采用包结结晶方法对小茴香挥发油中的对-丙烯基茴醚进行了选择性分离，以1,1,6,6-四苯基-2,4-已二炔-1,6-二醇(简称D.D)作为主体分子，小茴香挥发油中的对-丙烯基茴香醚作为客体分子，D.D选择性地与之形成超分子包结物晶体。采用IR,1^HNMR,单日XRD确定了包结物的形成及其主客体分子摩尔比为2:1。包结物晶体属于P1空间群，晶胞参数:a=1.2972(2)nm,b=1.5119(2)nm,c=1.6799(2)nm,α=100.57(1)°,β=104.89(1)°,γ=113.58(1)°,Z=2。利用Kugelrohr真空蒸馏技术从包结物晶体中蒸出被分离的化学组分，用IR，1^HNMR和MS方法，确定了反式对-丙烯基茴香醚。用GC方法测定了选择分离出的挥发油化学，GC分析结果表明，分离的反式对－丙烯基茴香醚的化学纯度为97%，回收率为75.28%。

关键词: 分子识别, 包结物, 结晶, 分离, 小荟香, 色谱质谱法, 丙烯基荟香醚

The chemical components of volatile oil from Foemiculum Vulgare Mill were determined by GC-MS. Anethole accounted for 82.65% of the whole oil. Selective isolation of anethole form the volatile oil was carried out using an inclusion crystalline method with 1,1,6,6- tetraphenylhexa- 2,4-diyne-1,6-diol inclusion complex with anethole . The crystal structure of the inclusion complex was determined by IR, 1^H NMR and single crystal XRD techniques. The host-guest molar ratio in complex was found to be 2:1. Crystal structure of inclusion compound belong to space group P1, a=1.2972 (2) nm, b=1.5119(2)nm, c=1.6799(2)nm, α=100.57(1)°,β=104.89(1)°,γ=113.58(1)°,Z=2. The isolated chemical component was isolated from the inclusion crystal complex by using Kugelrohr vacuum distillation technique and was identified to by trans-anethole by means of IR, 1^H NMR , and MS spectroscopy. The results of GC analysis showed that chemical purity of trans-anethole isolated from volatile oil was 97% and the yield was 75.28%.

Key words: OLECULAR RECOGNITION, CRYSTALLIZE, SEPARATION, CHROMATOGRAPHY-MASS SPECTROGRAPHY

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