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旋转膜乳化法制备尺寸均一的大粒径多糖微球
Alternative TitlePreparation of Uniform Large-sized Polysaccaride Beads by Rotating Membrane Emulsification
李小青
Subtype工程硕士
Thesis Advisor马光辉
2014-04
Degree Grantor中国科学院研究生院
Degree Discipline生物工程
Keyword旋转膜乳化法   琼脂糖微球   魔芋葡苷聚糖微球   大粒径
Abstract以琼脂糖和魔芋葡苷聚糖为基质制成的多糖微球可以开发成多种具有高附加值的产品,其中粒径在100微米左右及以上的微球有很多重要的应用,比如用作生物分离介质、医用血液净化吸附介质、细胞培养微载体等。 多糖凝胶微球的传统制备方法主要有机械搅拌法和喷射法等,然而这些传统方法制得的多糖微球粒径不均一、不可控,在使用前必须经过复杂的筛分过程,造成人力财力的极大浪费。本课题组在前期研究中,开发了可用于制备粒径在“几微米-百微米级”范围内的均一乳液及微球微囊的常规膜乳化技术。但是,常规膜乳化技术在用于制备粒径在百微米级及以上的均一微球时存在很多困难,乳滴在形成过程中极易聚并破乳,导致最终产品粒径不均一。 本论文将新型的旋转膜乳化技术引入到大粒径多糖(琼脂糖和魔芋葡苷聚糖)微球的制备中,探讨了大粒径均一多糖凝胶微球的制备工艺,以期开发出用于制备大粒径均一多糖微球产品的新型技术。论文工作主要包括以下四个部分:第一部分是搭建了旋转膜乳化装置,并通过简单乳液的制备对该装置进行了使用性能评价;第二部分是用旋转膜乳化技术制备均一的大粒径琼脂糖凝胶微球,系统考察了微球的制备工艺条件。通过考察水相琼脂糖浓度、油相液体石蜡/石油醚配比和膜管转速对琼脂糖凝胶微球的粒径及粒度分布均一性的影响,获得了制备均一大粒径琼脂糖凝胶微球的最佳制备工艺,成功制备出平均粒径为220 μm的均一琼脂糖凝胶微球,批次重复性相对标准偏差控制在2%以内。此外,还建立了旋转膜乳化技术制备大粒径琼脂糖凝胶微球机理的理论模型。利用响应面法以粒径均一性为基准分析了实验变量之间的相互影响,获得了实验参数的理论最优值;同时运用力学分析的方法以粒径尺寸为基准对旋转膜乳化技术制备琼脂糖凝胶微球的过程进行了理论分析,获得了琼脂糖乳滴粒径的理论预测计算模型。此部分获得的理论模拟工艺与第二部分工作中获得实际实验工艺相一致,进一步验证了所建理论模型的准确性;第三部分是对制得的大粒径琼脂糖凝胶微球进行化学交联,并且对制得的交联微球的耐热性、机械性能以及在分离纯化中的应用性能进行了系统评价;第四部分是用旋转膜乳化技术制备均一魔芋葡苷聚糖微球,系统考察了制备工艺参数,分析了旋转膜乳化技术在其他多糖体系的适用性。通过考察乳化剂种类、水相魔芋浆液的黏度、油相液体石蜡/石油醚配比和膜管转速对魔芋葡苷聚糖凝胶微球的粒径及其均一性的影响规律,获得了均一魔芋葡苷聚糖凝胶微球的最佳制备工艺,成功制备出平均粒径为70 μm的魔芋葡苷聚糖凝胶微球。 本论文的研究表明,旋转膜乳化技术能够有效解决大粒径多糖微球的制备问题,可应用于大粒径均一琼脂糖凝胶微球、均一魔芋葡苷聚糖凝胶微球以及其他体系乳液和微球的制备。
Other AbstractMany high value-added polysaccharide beads made from agarose and konjac glucomannan (KGM), especially, large-sized beads (around or more than 100 μm), have many important applications in biological separation medium, medical blood purification and cell culture carrier, etc. Traditional methods for preparation of polysaccharide gel beads mainly include mechanical mixing method and injection method. However, polysaccharide beads prepared by these traditional methods are mostly non-uniform, uncontrollable and need sieving before used, which will waste resources. Aiming at solving the problem of preparation of uniform emulsion droplets and microsphere with size range from 10 to 100 μm, our team has already developed cross-flow membrane emulsification. But this technology is less likely successful to prepare uniform droplets and microspheres with size around or above 100 μm. This dissertation introduced rotating membrane emulsification technology into preparation of uniform large-sized polysaccharide (from agarose and KGM) beads with size around or over 100 μm. This research mainly includes the following four parts:the first part was to build the rotating membrane emulsifier and investigate the performance of the emulsifier by preparing simple emulsion droplets;the second part focused on the preparation of uniform large-sized agarose beads by rotating membrane emulsification technology and the study of the control of preparation process. The optimum conditions for preparation of uniform large-sized agarose beads were obtained by investigating the effects of agarose concentration of water solution, volume ratio of liquid paraffin / petroleum ether in oil phase and rotational speed of the membrane tube on the size and uniformity of agarose bead. Uniform agarose beads prepared under the optimum conditions have an average size of 220 μm with good repeatability. The preparation of large-sized agarose beads by rotating membrane emulsification is theoretically simulated based on experimental results. The mutual effects between variables on the uniformity of beads and optimum values of the variables were investigated by the response surface methodology. And the forces of the procedure of rotating membrane emulsification were analyzed to obtain theoretical calculation formula of agarose emulsion droplet size. It was found that the experimental results in the second part were in accordance with the theoretical simulation values, which further verified the accuracy of the simulation; the third part focused on the chemical cross-linking of agarose beads and investigation of the performances of cross-linked beads, including thermal stability, mechanical stability and application in separation.; in the fourth part, rotating membrane emulsification was applied in preparation of other polysaccharide products, such as KGM beads. The optimum conditions for preparation of uniform KGM beads were obtained by investigating the effects of emulsifiers, viscosity of KGM solution, volume ratio of liquid paraffin / petroleum ether in oil phase and rotational speed of the membrane tube on the size and uniformity of KGM bead. Uniform KGM beads with average size of 70 μm were prepared under the optimum conditions. The studies in this dissertation show that rotating membrane emulsification technology can effectively solve the problem of preparation of uniform large-sized polysaccharide gel beads, such as agarose and KGM beads, and potentially be used to other system.
Language中文
Document Type学位论文
Identifierhttp://ir.ipe.ac.cn/handle/122111/15575
Collection研究所(批量导入)
Recommended Citation
GB/T 7714
李小青. 旋转膜乳化法制备尺寸均一的大粒径多糖微球[D]. 中国科学院研究生院,2014.
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