丁香酚-β-环糊精包合物的制备与表征
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篇名: 丁香酚-β-环糊精包合物的制备与表征
TITLE:
摘要:

目的:优化丁香酚-β-环糊精(β-CD)包合物的制备工艺,并对包合物进行鉴定和表征。方法:以丁香酚与β-CD的摩尔比、

包合温度、包合时间为考察因素,以包合率为评价指标,采用正交试验优选包合工艺并进行验证;采用红外光谱(FT-IR)、X-射线衍

射分析(XRD)和核磁一维氢谱(1H NMR)的谱图变化验证包合物的形成;通过核磁二维氢谱(1H ROESY NMR)表征包合物的结

构。结果:优选的制备工艺为丁香酚与β-CD 的摩尔比为1.0 ∶1,包合温度为60 ℃,包合时间为2.0 h;验证试验中平均包合率为

73.86%(RSD=0.17%,n=3)。包合物的1H NMR结果确定β-CD 与丁香酚包合物形成稳定结构时摩尔比为1.0 ∶1;FT-IR 和XRD

结果证实丁香酚与β-CD之间存在分子间相互作用力;1H ROESY NMR结果表明包合物的结构形式以丁香酚的苯环位于β-CD空

腔内、乙烯基位于β-CD空腔外为主。结论:所选工艺合理可行,可用于丁香酚与β-CD包合物的制备;波谱分析确证了包合物的形成。

ABSTRACT:

OBJECTIVE:To optimize the inclusion technology of Eugenol-β-cyclodextrin(β-CD)inclusion complex,and to

identify and characterize it. METHODS:With the molar ratio of eugenol to β-CD,inclusion temperature and inclusion time as factors,

using the yield of inclusion compounds as index,the inclusion technology was optimized by orthogonal test. The formation of

inclusion compound was identified by the spectra change of FT-IR,XRD and 1H NMR. Its structure was characterized by 1H ROESY

NMR. RESULTS:The optimized inclusion conditions were that the molar ratio of eugenol to β-CD was 1.0 ∶1;inclusion temperature

was 60 ℃;inclusion time was 2.0 h. And the yield of inclusion compound was 73.86%(RSD=0.17%,n=3). 1H NMR

results of β-CD and its inclusion complex indicated that the optimum qualitative ratio of the inclusion complex was 1.0 ∶1. The intermolecular

interaction between eugenol and β-CD was confirmed by the spectrum analysis of FT-IR and XRD. 1H ROESY NMR results

indicated the structure of inclusion complex mainly was that the phenyl of eugenol was in the cavity of β-CD,the vinyl was

outside. CONCLUSIONS:The inclusion technology is reasonable and feasible,and can be used for the inclusion of eugenol and

β-CD. The formation of inclusion compound is confirmed by the spectrum analysis.

期刊: 2016年第27卷第1期
作者: 朱庆英,张永辉,朱琼,丁乐
AUTHORS: ZHU Qingying,ZHANG Yonghui,ZHU Qiong,DING Le
关键字: 丁香酚;β-环糊精;包合物;制备;包合工艺;鉴定;表征
KEYWORDS: Eugenol;β-cyclodextrin;Inclusion complex;Preparation;Inclusion technology;Identification;Characterization
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