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The Study On Extraction, Purification And β-cyclodextrin Inclusion Of Nature D-borneol In Mei Pian Tree

Posted on:2017-05-10Degree:MasterType:Thesis
Country:ChinaCandidate:G D MeiFull Text:PDF
GTID:2271330503485005Subject:Light industrial technology and engineering
Abstract/Summary:PDF Full Text Request
D-Borneol has good pharmacological activities and distinctive flavor. So it has been used in many aeras, such as medicine, food, cosmetics, perfume and other industry. However, there are some problems need to be solved urgently in the production of D-Borneol. It is very important to study extraction techniques of the D-Borneol in order to get a more effective and efficient method for the industrial production of D-Borneol. Firstly, the crude D-Borneol was purified by using the method of recrystallization, then the morphology, thermodynamics and kinetics of the crystal were studied; D-Borneol-β-cyclodextrin inclusion complex was prepared and the stability and phase solubility of inclusion complex were analyzed. The results of this study could provide some theoretical and technical fundation for the industrial production and utilization of D-Borneol. The majorparts are listed as follows:1. Supercritical CO2 Extraction and Steam Distillation were applied to extract the volatile oil from the leaves and branches of the Mei Pian tree. The volatile oils extracted by two different methods were compared and analyzed by GC-MS. These results showed that the Supercritical CO2 Extraction method was better than the Steam Distillation method.2. The crude D-Borneol was recrystallized with petroleum ether, 120# gasoline and ethanol respectively, and the D-Borneol purity all increased significantly. After the recrystallization by petroleum ether and 120# gasoline, the crystal was in the shape of regular and platelike, while the crystal is irregular and granular shape after the recrystallization by anhydrous ethanol. Although the ethanol recrystallization was different with petroleum ether and 120# gasoline in morphology, the crystals obtained by the three methods were basically consistent with the standard in optical rotation and thermal properties. Besides, in the non-isothermal crystallization process of D-Borneol crystal, with the increase of cooling rate, the crystallization temperature decreases, and relative crystallinity both decreased, and crystallization time became shorter. In the same time, the crystallization rate with high crystallinity was higher than that with low crystallinity.3. Several embedding methods of inclusion complex of D-Borneol and β-Cyclodextrin were compared and we found that the ultrasonic method was superior to the saturated water solution method and grinding method. After optimization by orthogonal test, the optimum conditions of ultrasonic method were as follows: D-Borneol and β-Cyclodextrin feeding ratio was 1 : 6(g/g), the reaction time was 60 min, and the reaction temperature was 40?C. The structure of the inclusion complexes were characterized and analysised by DSC, XRD, FTIR and NMR. These results showed that the D-Borneol was already included in the cavity of cyclodextrin and inclusion complex was formed successfully. Moreover, the antivolatile and thermal stability antiphotolysis of D-Borneol in inclusion complexes were all improved, and the phase solubility curve of clathrate compound conformed as Bs type. Besides, the concentration of D-Borneol in water was increased with the concentration of cyclodextrin within a certain range and the solubility of D-Borneol was improved significantly.
Keywords/Search Tags:D-Borneol, Supercritical CO2 Extraction, recrystallized, β-cyclodextrin, inclusion complex
PDF Full Text Request
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