通常在N-琥珀酰壳聚糖的合成过程中使用大量的有毒溶剂,容易造成环境污染,并且有毒溶剂易残留在产物中,限制了N-琥珀酰壳聚糖在生物医学领域的应用。本研究采用一种安全、环保的合成方法,以无水乙醇为溶剂,通过控制反应时间,合成了一系列不同取代度的N-琥珀酰壳聚糖,测定了产物的取代度,分子量及其分布,并用FTIR对其进行结构分析。采用粉末X-射线衍射、TG对其结晶性能和热稳定性进行分析,并对其水溶性和生物相容性进行了探讨。当反应时间为15 h时,所得产物的取代度最高,分子量最大,分子量分布最窄;N-琥珀酰壳聚糖的结晶性和热稳定性均弱于壳聚糖,改性的壳聚糖具有良好的水溶性。动物皮下植入实验表明,以无水乙醇为溶剂合成的N-琥珀酰壳聚糖具有良好的生物相容性,有望在生物医用材料方面得到广泛应用。
Poisonous solvents were widely used in the preparation of N-succinyl-chitosan,which were easy to cause environmental pollution and difficult to remove completely from the products.These disadvantages limited their uses in biomedical materials.In the present work,a novel method was proposed to successfully synthesize N-succinyl-chitosan,which was safe and environmentally friendly.A series of N-succinyl-chitosan with different degrees of substitution were prepared in absolute ethanol by controlling the reaction time.The different degrees of substitution,molecular weight and polydispersity index of the products were measured.The products were characterized by Fourier transform infrared(FTIR) spectroscopy,X-ray diffractometry(XRD) and thermogravimetry(TG).Furthermore,the water-solubility and biocompatibility were studied.When the reaction time is 15 h,the degree of substitution and molecular weight of the product are highest.Moreover,polydispersity index of the product is smallest among all the products(10 h,12 h,15 h,18 h,20 h).In addition,the results indicate N-succinyl-chitosan has been synthesized with decreased degree of crystallization and thermostability.Water-solubility of modified chitosan is improved due to the decrease of crystallization.N-succinyl-chitosan prepared in absolute ethanol has good biocompatibility,which has great potential in biomedical fields.
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