相转移催化法制备羧甲基壳聚糖及其性能表征-食品科学.PDF

※工艺技术 食品科学 2009, Vol. 30, No. 06 39 肖玉良，李玉琴，夏成才，游桂荣，韩俊芬，段桂运，张海霞 (泰山医学院药学院，山东泰安 271000) 采用相转移催化法制备了羧甲基壳聚糖，考察了催化剂种类、催化剂使用量、反应温度、反应时间和 溶剂中水醇比对羧甲基壳聚糖取代度(DS) 和溶解性的影响。得到最佳反应条件为：以6% 的苄基三乙基氯化铵 (TEBA)作催化剂，反应温度55 ℃，反应时间4h ，溶剂中水醇比1:4(V/V)，羧甲基壳聚糖的取代度(DS)和溶解率 分别达到1.147 和98.87% 。并采用傅立叶红外光谱法及X 光电子能谱分析法对产物结构进行了表征，结果表明壳聚 糖羧甲基化反应主要是发生在C6 位上的－OH 基团上。 ：羧甲基壳聚糖；相转移催化；表征 Synthesis of Carboxymethyl Chitosan by Phase Transfer Catalytic Method and Its Characterization XIAO Yu-liang ，LI Yu-qin ，XIA Cheng-cai ，YOU Gui-rong ，HAN Jun-fen ，DUAN Gui-yun ，ZHANG Hai-xia (College of Pharmaceutical Sciences, Taishan Medical University, Taian 271000, China) Abstract ：In this study, preparation of carboxymethyl-chitosan (CMC) with phase transfer catalyst was described. Firstly, the effects of carboxymethylation conditions on the degree of substitution (DS) and solubility of CMC were investigated, and the optimum catalyst, reaction temperature, reaction time, volume ratio of water to alcohol are 6% of triethylbenzylammonium (TEBA), 55 ℃, 4 h and 1:4, respectively. Under these conditions, the DS and the solubility of CMC reach 1.147 and 98.87%, respectively. Then the chemical construction of CMC was characterized by Fourier-transformed infrared (FTIR) and X-ray photoelectron spectroscopy (XPS). The results showed that the carboxymethylation mainly occurs on hydroxy group in C6 site of chitosan. Key words ：carboxymethyl chitosan (CMC)；phase transfer catalysis ；characterization 中图分类号：Q063 文献标识码：A 文章编号：1002-6630(2009)06-0039-04 壳聚糖化学名称为(1,4)-2- 脱乙酰氨基-2- 脱氧- β-D 在微波催化下，用氯乙酸和壳聚糖在水溶液中反应，制 葡萄糖，是自然界储量极丰富的天然高分子碱性氨基多 得取代度0.85 的羧甲基壳聚糖。陈浩凡等[5]研究发现壳 糖，壳聚糖具有优良的生物相容性和生物可降解性，是 聚糖甲基化影响最大的因素为N a O H 用量，碱浓度过 理想的细胞