超声波合成羧甲基壳聚糖及表征

采用超声波辐射,以壳聚糖为原料、乙醇为分散介质、一氯乙酸为羧甲基化试剂合成了羧甲基壳聚糖,通过四因素三水平正交实验得出最优合成条件为：mNaOH/m壳聚糖为1．5;mclCH2COOH/m壳聚糖为1．5;反应时间2h;反应温度60℃;采用红外光谱仪、紫外-可见分光光度计、热重／差热分析仪、X射线衍射仪、扫描电镜对产物结构进行了表征．     

Study on volume ratio and plasticizer screening of free coating membranes composed of ethyl cellulose and chitosan

The aim of this study was to optimize the formula of free blended coating membrane of ethyl cellulose (EC) and chitosan (CS), including their suitable ratio range and the best plasticizer used. The dry films were produced by a casting/solvent evaporation method, with different volume ratio of EC and CS solution plasticized by various plasticizers, respectively. The wet films were prepared by immersing dry films in pH 6.8 phosphate buffer saline (PBS) for 24 h. The promising ratio range of EC/CS was below 20/5 or 20/6 with various plasticizer, which was determined by comparing the viscosity of the blended solutions and the morphology of the blended films. The efficiency of plasticization was evaluated by measuring glass transition temperature (T_g). All the testing plasticizers have good compatibility with EC or CS and dibutyl phthalate (DBP) have the strongest efficiency inducing the lowest T_g (39.9°C) of the film. Mechanical properties were evaluated by the ratio of tensile strength (T) to elastic modulus (E). In the wet state, the films with DBP had the highest T/E value (1.2). The results of leaching of plasticizers also verified that DBP was the most stable plasticizer in the films. The release rates of tetramethylpyrazine phosphate (TMPP) through the pellets coated with the blended films of EC/CS (20 : 6 v/v) plasticized by various plasticizers showed that the more water‐soluble the plasticizer was, the more quickly TMPP dissolved from the coated pellets, which further indicated that the water‐insoluble plasticizers (such as DBP) could be more applicable to keep the sustained or controlled release property of the blended films in wet state. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 1932–1939, 2006     

球型Co2+印迹壳聚糖树脂的吸附特性及动力学研究

以Co2 和壳聚糖为原料,环氧氯丙烷和异丙醇为交联剂,制备了球形Co2 印迹壳聚糖树脂。研究了pH值、温度等因素对该印迹树脂吸附的影响及其吸附动力学。结果表明,pH值小于3.5时,印迹CTS树脂无吸附能力,pH值在3.5～6.0之间,印迹CTS树脂的吸附量随pH值升高而增大。印迹CTS树脂的吸附符合二级吸附动力学方程:t/Q=0.0077 0.0048 t。球形印迹壳聚糖树脂的吸附是以多分子层不均匀吸附模式为主,符合Freundlich方程。在30～90℃的温度范围内,树脂的吸附量随温度升高而增加,70℃时达到最大值,随后呈下降趋势。     

阿司匹林壳聚糖纳米缓释微球的制备及体外释放性能的研究

以自制阿司匹林为药物,壳聚糖为载体,采用乳化-化学交联法制备了阿司匹林-壳聚糖载药微球,确定了阿司匹林-壳聚糖载药微球的制备工艺条件,探讨搅拌速度、阿司匹林/壳聚糖质量比、交联剂戊二醛、乳化剂Span-80用量对微球的药物包封率、载药量和释药性能的影响。研究结果表明,室温条件下,以液体石蜡为介质,选用3%的壳聚糖冰醋酸溶液、按阿司匹林∶壳聚糖=1.5∶1、4%的戊二醛为交联剂、Span-80用量为体积比6%、中等搅拌速度制备出的微球药物包封率可达79%,微球粒径最小可达20 nm,制得的载药微球在16 h内对药物有良好的缓释作用,在25 h之内仍存在缓药效果。     

两种壳聚糖降解工艺的比较研究

比较了NaNO2/HAc与H2O2/HAc两种体系降解壳聚糖工艺,探讨了反应时间、NaNO2及H2O2用量、醋酸质量分数、壳聚糖浓度等因素在不同体系下对降解速度及壳聚糖分子量的影响.结果表明,NaNO2/HAc体系最佳降解条件为:降解温度30℃、醋酸质量分数5%、壳聚糖浓度0.02 g·mL-1、NaNO2体积0.20 mL、降解时间45 min,降解所得到的低聚壳聚糖平均分子量约为1.7×104.H2O2/HAc体系最佳降解条件为:降解时间4 h、降解温度60℃、醋酸质量分数5%、壳聚糖浓度0.02 g·mL-1、30%H2O2体积0.50 mL,降解所得到的低聚壳聚糖平均分子量约为2.1×104.     

棉织物的抗菌免烫整理研究

通过正交试验探讨了用H2 O2 氧化降解法制备适用于与聚羧酸MAA - 1配合进行抗菌免烫整理的低聚水溶性壳聚糖的最佳工艺 ,研究了降解壳聚糖与聚羧酸MAA - 1配合对棉织物进行抗菌免烫整理的工艺以及降解壳聚糖的质量浓度和相对分子质量对整理效果的影响。结果表明 :用 80g/L的聚羧酸MAA - 1和 4 0 g/L相对分子质量为 90 0 0的降解壳聚糖分两浴整理的棉织物的褶皱回复角为 2 71°,DP等级为 4 .0 ,断裂强力保留率为 6 4 % ,对大肠杆菌和金黄色葡萄球菌的抗菌率分别为 94%和 83%。经过 2 0次洗涤 ,其WRA为 2 5 7° ,DP等级为 3.7,而抗菌率则均保持在洗涤前的 80 %以上。阴离子染料 (直接冻黄G)染色的K/S值较用聚羧酸MAA - 1整理的棉织物提高了 1 .85。     

Synthesis and properties of chitosan-modified poly(vinyl butyrate)

Modification of chitosan by grafting of vinyl butyrate was carried out in homogeneous phase using potassium persulfate as redox initator and 1.5% acetic acid as solvent. The percent grafting and grafting efficiency were analysed and the high grafting efficiency up to 94% was observed. The effects of reaction variables such as monomer concentration, initiator concentration, temperature and reaction time were investigated. It was observed that the solubility of chitosan was markedly reduced after grafting with vinyl butyrate. The grafted product is insoluble in common organic solvents as well in dilute organic and inorganic acids. Characterization of the graft copolymers were carried out by using Fourier Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC) and Scanning Electron Microscopy (SEM) technics. Characteristic signal of carbonyl group was observed at 1,731 cm⁻¹ which belongs to the poly vinyl butyrate segments in the graft copolymer. The melting transition of the chitosan main chain in the copolymer shifted to 124°C from its original value 101°C. In addition to these, we have also studied topology of the graft copolymer and the SEM micrograph showed continuous homogenous matrix which means there is no phase separation.     

天然高分子壳聚糖在环保领域中的研究及应用

综述了壳聚糖在水处理、大气污染治理、减轻水果蔬菜农药污染以及在制备生物降解材料上的应用及研究进展。     

Periodontal ligament cells cultured on the tricalcium phosphate/chitosan scaffolds in vivo and in vitro

To search suitable scaffolds for periodontal tissue regeneration, different ratios of tricalcium phosphate/chitosan(TCP/chitosan) scaffolds were prepared through a freeze-drying process. Human periodontal ligament cells(HPLCs) were incubated on the scaffolds in vitro. Cells were cultured on the scaffolds, detected by scanning electron microscopy (SEM). HPLCs were analyzed by MTT assay and alkaline phosphatase(ALP) activity detection. HPLCs were seeded onto the scaffolds. Then these scaffolds with HPLCs were implanted subcutaneously into athymic mice. The state of periodontal tissue regeneration was detected after 4 weeks. As the ratio of TCP increased, TCP/chitosan scaffolds accelerated HPLCs proliferation significantly higher than the pure chitosan scaffold. HPLCs produced the cementoid tissue in vivo. The periodontal tissue regeneration engineering is able to be applied with TCP/chitosan scaffolds.     

Evaluation of apatite-coated chitosan microspheres for bone regeneration

The apatite-coated chitosan microspheres were fabricated by incubating chitosan in five times simulated body fluid. The apatite deposited on the microspheres was similar to natural bone mineral, as demonstrated by scanning electron microscopy, X-ray diffraction spectra and Fourier transformed-infrared spectroscopy analyses. Rat bone marrow-derived mesenchymal stem cells （BMSCs） were seeded on apatite- coated microspheres to investigate the effect of this scaffold on cell proliferation and differentiation. BMSCs seeded on uncoated microspheres were served as a control. In vivo experiment was evaluated by transplanting the microspheres loaded with or without BMSCs in 5-mm cranial defects of Wistar rats. Bone regeneration was investigated via micro-CT and histological analysis. It was found that apatite-coated chitosan microspheres could significantly promote the proliferation and alkaline phosphatase activity of BMSCs compared with uncoated microspheres. Histological slices and Micro-CT images at 8 weeks revealed much better regeneration of bone in the apatite-coated microspheres loaded with BMSCs than the control. In addition, the defect filled with pure microspheres induced little new bone formation. Our findings suggest that the apatite-coated chitosan microspheres scaffold is a promising carrier of stem cells for cranial bone tissue engineering.