阴离子淀粉基多孔树脂的设计合成及其对喜树碱吸附分离行为

Research and development of green and safe adsorptive separation resin has important scientific significance and practical value for the extraction of active ingredients from the traditional Chinese medicine. The aim of this project is to design and synthesis of a new class of green adsorptive separation materials based starch. Firstly, three soluble anionic starches, including carboxymethyl starch, starch phosphate and starch sulfate, are prepared by using starch as a raw material, and then the porous resins based anionic starch are prepared from anionic starch by emulsifying-curing method under the porogen. Polyethylene glycol and epichlorohydrin are used as polymer crosslinkers to improve the strength and polarity of the porous resin based anionic starch. The particle size of the resin is controlled to 20 to 60 mesh by optimizing the crosslinker and the emulsion systems. The environment-friendly porogens are chosen to regulate the porous morphology of the resin. The structure, morphology and characteristic parameters of the resin as an adsorptive separation material are characterized. The adsorptive separation behavior of camptothecin by the resin is examined by using static batch and dynamic column adsorption methods. The adsorption kinetics, the adsorption thermodynamics and the adsorption equilibrium models are built, and the elution of the camptothecin from the resin is also studied. The structure and morphology of the resin, which affect on its adsorptive separation performance of the camptothecin, are revealed to lay the foundation for the resin to be used as an adsorptive separation material.

研制和开发绿色安全型吸附分离树脂对中药有效成分的提取分离具有重要的科学意义和实用价值。本项目旨在设计合成一类新型的淀粉基绿色吸附分离材料。以淀粉为原料，首先在淀粉分子中引入羧基、磷酸基或硫酸基制备水溶性阴离子淀粉，再在致孔剂作用下通过乳化-交联固化法制备阴离子淀粉基多孔树脂。通过聚乙二醇与环氧氯丙烷构成的长链交联体系调控阴离子淀粉基树脂的强度和极性；再结合乳化体系的优化调控树脂的粒径在20～60目；选择环境友好的致孔剂构筑树脂的多孔形态。系统表征阴离子淀粉基多孔树脂的结构形态及其作为吸附分离材料的特征参数，通过静态分批法和动态柱吸附法研究树脂对喜树碱的吸附分离行为；建立阴离子淀粉基多孔树脂对喜树碱的吸附动力学、吸附热力学以及吸附平衡模型，系统研究喜树碱在树脂上的洗脱行为。揭示阴离子淀粉基多孔树脂的结构形态影响其吸附分离喜树碱的规律，为其用作吸附分离材料奠定一定的理论基础。

研制和开发绿色安全型吸附分离树脂对中药有效成分的提取分离具有重要的科学意义和实用价值。本项目设计合成一类新型的淀粉基绿色吸附分离材料。以淀粉为原料，首先在淀粉分子中引入羧基、磷酸基或硫酸基制备水溶性阴离子淀粉，再在致孔剂作用下通过乳化-交联固化法制备阴离子淀粉基多孔树脂。通过聚乙二醇与环氧氯丙烷构成的长链交联体系调控阴离子淀粉基树脂的强度和极性；再结合乳化体系的优化调控树脂的粒径在20～60目；选择环境友好的致孔剂构筑树脂的多孔形态。系统表征阴离子淀粉基多孔树脂的结构形态及其作为吸附分离材料的特征参数，通过静态分批法和动态柱吸附法研究树脂对喜树碱的吸附分离行为；建立阴离子淀粉基多孔树脂对喜树碱的吸附动力学、吸附热力学以及吸附平衡模型，系统研究喜树碱在树脂上的洗脱行为。磷酸淀粉酯多孔树脂对喜树碱表现出最佳的吸附性能。吸附动力学和吸附平衡分别遵循假定一级动力学模型和Langmuir模型。从Langmuir模型拟合中可以得到293K时最大吸附量为0.60mmol/g。动态柱吸附实验结果表明，经过5次吸附解吸循环应用后，磷酸淀粉酯多孔树脂对喜树碱的吸附量有所下降，但仍然保持在一个比较高的水平。揭示阴离子淀粉基多孔树脂的结构形态影响其吸附分离喜树碱的规律，为其用作吸附分离材料奠定一定的理论基础。