羧甲基马铃薯淀粉的制备、反应动力学及性能研究
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摘要
本学位论文以马铃薯淀粉为原料,分别在两种不同的反应介质中制备了羧甲基淀粉,对其反应条件进行了优化。同时,对马铃薯淀粉羧甲基化反应动力学、羧甲基淀粉水溶液性质、离子交联的壳聚糖-羧甲基淀粉水凝胶的pH值敏感性及其载药凝胶的释药行为进行了研究。得到的主要结果有:
(1)在异丙醇溶剂中制备了高取代度和高反应效率的羧甲基马铃薯淀粉,探讨了醚化反应温度、碱化反应时间、醚化反应时间、氢氧化钠与一氯乙酸的摩尔比、一氯乙酸与马铃薯淀粉分子中脱水葡萄糖单元的摩尔比以及异丙醇体积与马铃薯淀粉质量之比对马铃薯淀粉羧甲基化过程的影响,得出了该方法制备羧甲基马铃薯淀粉的最佳反应条件。利用傅立叶变换红外光谱仪表征了产物的结构,使用扫描电子显微镜观察了马铃薯淀粉羧甲基化前后表面形貌的变化,并运用铜盐沉淀法测定了羧甲基马铃薯淀粉的取代度。
(2)在乙醇-水混合溶剂中制备了羧甲基马铃薯淀粉,并运用正交实验设计,以羧甲基淀粉取代度和2%水溶液表观粘度为指标,对反应条件进行了优化。优化条件包括:氢氧化钠的加入次数、淀粉与溶剂的混合时间、醚化反应温度、碱化反应时间、混合溶剂中水的含量、混合溶剂体积与马铃薯淀粉质量之比、氢氧化钠与一氯乙酸的摩尔比以及一氯乙酸与马铃薯淀粉分子中脱水葡萄糖单元的摩尔比。用傅立叶变换红外光谱仪表征了产物的结构,用分光光度法和旋转粘度计分别测定了羧甲基马铃薯淀粉的取代度和2%水溶液表观粘度。
(3)探讨了马铃薯淀粉在甲醇-异丙醇混合溶剂中的羧甲基化反应动力学,建立了反应动力学方程,得出了速率常数。采用X射线衍射分析仪研究了在不同的反应介质中羧甲基化过程对马铃薯淀粉结晶结构的影响,用示差扫描量热仪比较了马铃薯淀粉和羧甲基马铃薯淀粉的玻璃化转变温度。
(4)研究了各种外在因素对羧甲基马铃薯淀粉水溶液表观粘度的影响,如羧甲基淀粉水溶液的浓度、搅拌时间、甘油体积百分比、葡萄糖含量、魔芋葡甘聚糖含量、各种不同的氯化物、溶解顺序和温度以及剪切速率等。
(5)采用离子交联法制备了壳聚糖-羧甲基淀粉水凝胶,考察了其在不同的缓冲溶液中的溶胀情况。在此基础上,以维生素B1为模型药物,研究了载药壳聚糖-羧甲基淀粉交联凝胶在模拟十二指肠液中的药物释放行为。利用傅立叶变换红外光谱仪分析了药物分子与聚合物之间以及聚合物与聚合物之间的相互作用。
In this thesis, carboxymethyl potato starch was synthesized respectively in two different reaction media and the factors affecting the process of reactions were investigated systematically. Moreover, the kinetics of carboxymethylation on potato starch and solution properties of carboxymethyl starch aqueous solution were studied. In addition, ionic crosslinked chitosan-carboxymethyl starch gel beads were prepared and the drug release behaviors of drug-loaded beads were researched in simulation duodenal fluid. The main results were summarized as follows:
(1) Carboxymethyl potato starch was synthesized in isopropanol solvent. The influences of etherification temperature, alkalization and etherification time, sodium hydroxide to monochloroacetic acid molar ratio, monochloroacetic acid to anhydroglucose units in starch molar ratio, the ratio of isopropyl alcohol volume to starch mass on degree of substitution and reaction efficiency of carboxymethyl starch were investigated. And the optimal reaction conditions for the carboxymethyl potato starch were obtained. Moreover, potato starch and carboxymethyl potato starch were characterized by Fourier transform infrared spectrophotometer and scanning electron microscope. In addition, the degree of substitution of carboxymethyl starch was determined by copper salt precipitation method.
(2) Optimization of preparation conditions of carboxymethyl potato starch was carried out through orthogonal experimental design in the solvent of ethanol-water mixture. The effects of relevant factors on the apparent viscosity of 2% carboxymethyl starch aqueous solution and degree of substitution were investigated. These condition parameters included charging times of sodium hydroxide, mixing time of starch and solvent, etherification temperature, alkalization time, water content in the mixed solvent, ratio of liquid volume to starch mass, molar ratio of sodium hydroxide to monochloroacetic acid and molar ratio of monochloroacetic acid to anhydroglucose unit in starch. Furthermore, potato starch and carboxymethyl potato starch were characterized by Fourier transform infrared spectrophotometer. And the apparent viscosity of 2% carboxymethyl starch aqueous solution and degree of substitution were measured by the J acid colorimetric method and by NDJ-1 viscometer, respectively.
(3) The kinetics of starch carboxymethylation in methanol, isopropanol and methanol-isopropanol mixtures was explored and carboxymethyl kinetic equation was established. The influence of carboxymethyl process on crystalline structure of potato starch was studied by X-ray diffractometer. And the glass transition temperatures of potato starch and carboxymethyl potato starch were determined using a sapphire differential scanning calorimeter.
(4) The viscosity behaviors of CMS aqueous solution were researched. The dependences of apparent viscosity of CMS aqueous solution on concentration of CMS aqueous solution, stirring time, glycerin, glucose, konjac glucomannan, seven low molecular weight electrolytes, dissolving sequence and temperature, and shear rate were investigated. The results showed that these factors had very different effect on apparent viscosity of CMS aqueous solution.
(5) Chitosan-carboxymethyl starch gel beads (CSCM) were prepared using sodium tripolyphosphate as an ionic crosslinker. And swelling experiments were performed by immersed about 50 mg dried CSCM in 50 ml buffer solutions with different pH values at 37±1℃. Moreover, in vitro release of model drug from these beads obtained under different reaction conditions was studied in simulation duodenal fluid. In addition, the interaction between drug (or polymer) and polymer was characterized by Fourier transform infrared spectrophotometer.
(1)在异丙醇溶剂中制备了高取代度和高反应效率的羧甲基马铃薯淀粉,探讨了醚化反应温度、碱化反应时间、醚化反应时间、氢氧化钠与一氯乙酸的摩尔比、一氯乙酸与马铃薯淀粉分子中脱水葡萄糖单元的摩尔比以及异丙醇体积与马铃薯淀粉质量之比对马铃薯淀粉羧甲基化过程的影响,得出了该方法制备羧甲基马铃薯淀粉的最佳反应条件。利用傅立叶变换红外光谱仪表征了产物的结构,使用扫描电子显微镜观察了马铃薯淀粉羧甲基化前后表面形貌的变化,并运用铜盐沉淀法测定了羧甲基马铃薯淀粉的取代度。
(2)在乙醇-水混合溶剂中制备了羧甲基马铃薯淀粉,并运用正交实验设计,以羧甲基淀粉取代度和2%水溶液表观粘度为指标,对反应条件进行了优化。优化条件包括:氢氧化钠的加入次数、淀粉与溶剂的混合时间、醚化反应温度、碱化反应时间、混合溶剂中水的含量、混合溶剂体积与马铃薯淀粉质量之比、氢氧化钠与一氯乙酸的摩尔比以及一氯乙酸与马铃薯淀粉分子中脱水葡萄糖单元的摩尔比。用傅立叶变换红外光谱仪表征了产物的结构,用分光光度法和旋转粘度计分别测定了羧甲基马铃薯淀粉的取代度和2%水溶液表观粘度。
(3)探讨了马铃薯淀粉在甲醇-异丙醇混合溶剂中的羧甲基化反应动力学,建立了反应动力学方程,得出了速率常数。采用X射线衍射分析仪研究了在不同的反应介质中羧甲基化过程对马铃薯淀粉结晶结构的影响,用示差扫描量热仪比较了马铃薯淀粉和羧甲基马铃薯淀粉的玻璃化转变温度。
(4)研究了各种外在因素对羧甲基马铃薯淀粉水溶液表观粘度的影响,如羧甲基淀粉水溶液的浓度、搅拌时间、甘油体积百分比、葡萄糖含量、魔芋葡甘聚糖含量、各种不同的氯化物、溶解顺序和温度以及剪切速率等。
(5)采用离子交联法制备了壳聚糖-羧甲基淀粉水凝胶,考察了其在不同的缓冲溶液中的溶胀情况。在此基础上,以维生素B1为模型药物,研究了载药壳聚糖-羧甲基淀粉交联凝胶在模拟十二指肠液中的药物释放行为。利用傅立叶变换红外光谱仪分析了药物分子与聚合物之间以及聚合物与聚合物之间的相互作用。
In this thesis, carboxymethyl potato starch was synthesized respectively in two different reaction media and the factors affecting the process of reactions were investigated systematically. Moreover, the kinetics of carboxymethylation on potato starch and solution properties of carboxymethyl starch aqueous solution were studied. In addition, ionic crosslinked chitosan-carboxymethyl starch gel beads were prepared and the drug release behaviors of drug-loaded beads were researched in simulation duodenal fluid. The main results were summarized as follows:
(1) Carboxymethyl potato starch was synthesized in isopropanol solvent. The influences of etherification temperature, alkalization and etherification time, sodium hydroxide to monochloroacetic acid molar ratio, monochloroacetic acid to anhydroglucose units in starch molar ratio, the ratio of isopropyl alcohol volume to starch mass on degree of substitution and reaction efficiency of carboxymethyl starch were investigated. And the optimal reaction conditions for the carboxymethyl potato starch were obtained. Moreover, potato starch and carboxymethyl potato starch were characterized by Fourier transform infrared spectrophotometer and scanning electron microscope. In addition, the degree of substitution of carboxymethyl starch was determined by copper salt precipitation method.
(2) Optimization of preparation conditions of carboxymethyl potato starch was carried out through orthogonal experimental design in the solvent of ethanol-water mixture. The effects of relevant factors on the apparent viscosity of 2% carboxymethyl starch aqueous solution and degree of substitution were investigated. These condition parameters included charging times of sodium hydroxide, mixing time of starch and solvent, etherification temperature, alkalization time, water content in the mixed solvent, ratio of liquid volume to starch mass, molar ratio of sodium hydroxide to monochloroacetic acid and molar ratio of monochloroacetic acid to anhydroglucose unit in starch. Furthermore, potato starch and carboxymethyl potato starch were characterized by Fourier transform infrared spectrophotometer. And the apparent viscosity of 2% carboxymethyl starch aqueous solution and degree of substitution were measured by the J acid colorimetric method and by NDJ-1 viscometer, respectively.
(3) The kinetics of starch carboxymethylation in methanol, isopropanol and methanol-isopropanol mixtures was explored and carboxymethyl kinetic equation was established. The influence of carboxymethyl process on crystalline structure of potato starch was studied by X-ray diffractometer. And the glass transition temperatures of potato starch and carboxymethyl potato starch were determined using a sapphire differential scanning calorimeter.
(4) The viscosity behaviors of CMS aqueous solution were researched. The dependences of apparent viscosity of CMS aqueous solution on concentration of CMS aqueous solution, stirring time, glycerin, glucose, konjac glucomannan, seven low molecular weight electrolytes, dissolving sequence and temperature, and shear rate were investigated. The results showed that these factors had very different effect on apparent viscosity of CMS aqueous solution.
(5) Chitosan-carboxymethyl starch gel beads (CSCM) were prepared using sodium tripolyphosphate as an ionic crosslinker. And swelling experiments were performed by immersed about 50 mg dried CSCM in 50 ml buffer solutions with different pH values at 37±1℃. Moreover, in vitro release of model drug from these beads obtained under different reaction conditions was studied in simulation duodenal fluid. In addition, the interaction between drug (or polymer) and polymer was characterized by Fourier transform infrared spectrophotometer.
引文
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