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Alternative TitlePreparation and stability study of crocin and crocetin microcapsules
Thesis Advisor袁晓凡
Degree Grantor中国科学院研究生院
Degree Discipline生物化工
Keyword高速逆流色谱   喷雾干燥   稳定性   西红花苷   西红花酸
Abstract对中药栀子中的西红花苷和西红花酸进行了制备及稳定性研究,用高速逆流色谱制备了纯度为96.6%的西红花苷,探讨了西红花苷苷元(西红花酸)的稳定性影响因素,并首次用喷雾干燥制备微胶囊技术成功改善了西红花酸稳定性,使其半衰期延长至3.2倍,并对该胶囊进行了动力学和热力学稳定性分析及形态表征。主要结论如下:高速逆流色谱可以用来分离西红花苷,正丁醇/水溶剂系统较其它系统更合适。正丁醇/乙酸乙酯/水(20:1:20)溶剂系统对西红花苷分配系数(1.05)接近1.0,分层时间为19s;在800 r/min时,仪器固定相保留率为43%,满足分离要求;分离得到了13 mg西红花苷粉末,纯度经液相检测达96.6%,单步回收率10%。研究了西红花酸的稳定性,发现它受多个外部因素的影响。影响的强弱顺序为光照>氧气>温度。采用喷雾干燥技术制备西红花酸微胶囊,最优工艺条件为进风温度195℃、液固比30:1、膜/核比5:1,在使用的三种微胶囊包埋材料(β-环糊精、阿拉伯胶和麦芽糖糊精)中,阿拉伯胶最为理想。对西红花酸微胶囊粉末的形态学分析表明喷雾干燥形成了良好的胶囊结构,其粒径分布受乳浊液粘度影响很大,阿拉伯胶包埋的微胶囊平均粒径为475.1 nm。微胶囊化能有效提高西红花酸稳定性。研究表明西红花酸降解很好地服从一级动力学反应(R2>0.9),β-环糊精、 阿拉伯胶和 麦芽糖糊精作为膜材料能将西红花酸半衰期分别提高至1.3倍、2.1倍和3.2倍。在进风温度210℃、液固比10:1和相对湿度0.75条件下,β-环糊精、 阿拉伯胶和 麦芽糖糊精这三种微胶囊膜对氧气传递的活化能分别为29.448±0.080 kJ/mol,58.847±0.312 kJ/mol及49.391±0.125 kJ/mol,表明阿拉伯胶膜材料屏蔽氧气的能力最强。
Other AbstractPreparation and stability studies of crocin and crocetin in Chinese herbal medicines Gardenia were investigated in this thesis. Crocin with a purity of 96.6% was prepared by high-speed countercurrent chromatography method. The main factors affecting the stability of crocin aglycone (crocetin) was investigated. The half-time of crocetin was prolonged to 3.2 times with the help of microcapsules formed by spray drying. Then the thermodynamic and kinetic analysis on the stabilities of these microcapsules and the morphology characteristics were analysed. The main conclusions were as follows: 1) High-speed countercurrent chromatography can be used in crocin separation. The crocin distribution coefficient (1.05) was close to 1.0 and the hierarchical time was 19 s in the most suitable solvent system n-butanol / ethyl acetate / water ( 20:1:20); The stationary phase retention rate in the instrument was 43% at 800 r/min, which met the separation requirements. The purity of the crocin powder obtained under the above conditions reached 96.6% and the single-step recovery rate reached 10%. 2) The stability of crocetin was affected by many factors ( light > oxygen > temperature). The optimum conditions for the preparation of crocetin microcapsule by spray drying were as follows: the inlet air temperature of 195 °C, liquid to solid ratio of 30:1, membrane to nuclear ratio of 5:1. Gum arabic was the most ideal material among the three materials used. 3) Microencapsulation can effectively improve the stability of crocetin. Studies showed that the degradation of crocetin followed the first-order reaction kinetics model (R2> 0.9). With β-cyclodextrin, gum arabic and maltodextrin as wall materials, the half-life of crocetin in microcapsules was prolonged to 1.3, 2.1 and 3.2 times respectively. The morphology analysis of crocetin microencapsulated powder showed that spray drying was suitable to form good microcapsule structure and the particle size distribution was affected greatly by the viscosity of the emulsions. Average particle diameter of gum arabic microcapsule powders was 475.1 nm. 4) The ability of oxygen shielding was affected by the spray drying process and storage conditions. Under the inlet air temperature 210 ° C, the liquid to solid ratio 10:1 and a storage relative humidity 0.75, the activation energy of oxygen transfer through the three microcapsule membranes formed by β-cyclodextrin, gum arabic and maltodextrins were 29.448 ± 0.080 kJ/mol, 58.847 ± 0.312 kJ/mol and 49.391 ± 0.125 kJ/mol respectively, 
Document Type学位论文
Recommended Citation
GB/T 7714
周辉. 西红花苷和西红花酸微胶囊的制备及稳定性研究[D]. 中国科学院研究生院,2013.
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