壳寡糖及其金属离子配合物的合成研究

发布时间：2017-12-27 19:27

本文关键词：壳寡糖及其金属离子配合物的合成研究　出处：《天津工业大学》2017年硕士论文　论文类型：学位论文

【摘要】：壳寡糖(Chitooligosaccharides,简称COS)是从虾蟹类生物外壳的甲壳素中提取,由2-10个氨基葡萄糖通过β-1,4糖苷键连接而成的低分子量壳聚糖。作为自然界中唯一带正电荷、呈碱性、水溶性的多糖,壳寡糖不仅具有相对分子量小和可溶性高等优点,而且还拥有许多独特的生理活性和功能性质。壳寡糖分子中含有大量的羟基和氨基,它可以依靠氢键或盐键形成具有类似网状结构的笼形分子,极易和金属离子发生配位反应生成壳寡糖金属配合物,而这类配合物不仅具有壳寡糖的优良性能,而且拥有金属离子的相关特性,被广泛应用于保健食品生产与开发,金属分离及含量检测、生物医药等领域。因此,壳寡糖金属配合物具有重要的研究意义和实际应用价值。本文研究了过氧化氢氧化制备壳寡糖的方法,考察了反应温度、时间以及过氧化氢浓度对降解效果的影响,并对所得产物进行了粘均分子量测定,从而得到最佳的制备工艺条件为反应温度60℃,反应时间6小时,过氧化氢质量分数3%,在此条件下制得壳寡糖的粘均分子量为2.11×103左右;除此之外,本文合成了三种壳寡糖金属配合物,分别是壳寡糖铁配物(COS-Fe)、壳寡糖铜配物(COS-Cu)和壳寡糖镍配物(COS-Ni)。利用紫外光谱和红外光谱对产物进行了表征分析,从而证实了所得产品即为壳寡糖金属元素的配位产物,确定了和金属离子Fe3+、Cu2+、Ni2+配位的优化条件为配位溶液的pH值应控制在4-5左右,综合虑到实际工业生产中的生产周期和能量损耗等条件,反应时间应该控制在60min左右,反应温度控制在40-50℃;通过对壳寡糖金属配位产物的热重分析和元素分析,不仅证实了配位产物的存在,而且确定了壳寡糖和金属离子进行配位时的摩尔比值,通过测试数据的计算可以推断出壳寡糖和铁(Ⅲ)元素配位比值为3:1,壳寡糖和铜(Ⅱ)元素配位比值为2:1,壳寡糖和镍(Ⅱ)元素配位比值为3:1。
[Abstract]:Chitosan oligosaccharide (Chitooligosaccharides, referred to as COS) is extracted from crab shell chitin biological, low molecular weight chitosan which are connected by 2-10 through -1,4 glucosamine beta glycosidic bond. As the only natural polysaccharide with positive charge, alkaline and water-soluble, chitosan oligosaccharide has not only the advantages of relatively small molecular weight and high solubility, but also has many unique physiological and functional properties. The chitosan oligosaccharide molecule contains a large number of hydroxyl groups and amino groups, it can rely on hydrogen bonds or salt bond formation with similar mesh structure of Cryptophane easily, and metal ion coordination reaction of chitosan metal complexes, such complexes not only has excellent performance of chitosan, and has characteristics of metal ions which is widely used in health food production and development, metal separation and content detection, biomedicine and other fields. Therefore, the metal complexes of chitosan oligosaccharides have important research significance and practical application value. This paper studies the method for the oxidation of hydrogen peroxide preparation of chitooligosaccharides. The effects of reaction temperature, time and concentration of hydrogen peroxide on the degradation effect, and the products were analyzed by viscosity average molecular weight determination, in order to get the optimal preparation conditions for the reaction temperature is 60 DEG C, the reaction time of 6 hours, 3% mass fraction of hydrogen peroxide, this prepared under the condition of chitosan oligosaccharide viscosity average molecular weight is about 2.11 * 103; in addition, three kinds of chitosan metal complexes were synthesized in this paper, chitosan iron complexes (COS-Fe), chitosan copper complexes (COS-Cu) and chitosan (COS-Ni) nickel complexes. The products were characterized by ultraviolet spectroscopy and infrared spectroscopy, which confirmed that the product is chitosan metal elements coordination product was determined and the metal ions of Fe3+, Cu2+, Ni2+ with the optimized conditions for the coordination of the pH value of the solution should be controlled at around 4-5, according to the actual comprehensive industrial production in the production cycle and energy loss and other conditions, the reaction time should be controlled at around 60min, the reaction temperature is controlled at 40-50 DEG C; the chitosan metal coordination product of thermogravimetric analysis and elemental analysis, not only confirmed the existence of product coordination, and to determine the chitosan and metal ions with a molar ratio when, through the calculation of test data can be inferred that oligochitosan and iron (III) element coordination ratio is 3:1, chitosan and copper (II) element coordination ratio is 2:1, chitosan and nickel (II) element coordination ratio is 3:1.
【学位授予单位】：天津工业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O641.4

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