【摘要】 目的制备羧甲基几丁质并对其性能进行研究。方法以新鲜虾壳为原料制备几丁质,然后采用碱化和醚化反应以及提纯工艺制备羧甲基几丁质。采用双突跃电位滴定法测定脱乙酰度、元素分析法测定取代度、傅立叶变换红外光谱仪和核磁共振仪分析羧甲基的取代位置,采用凝胶色谱结合多角激光光散射仪测定相对分子质量及其分布,并按照GB/T16886医疗器械生物学评价对其生物学性能进行检测。结果通过将新鲜虾壳进行脱钙和去除蛋白质后制备的几丁质进行碱化和醚化反应可成功制备羧甲基几丁质。采用双突跃电位滴定法测得羧甲基几丁质的脱乙酰度为13.76%,采用元素分析法测得的脱乙酰度和取代度分别为14.53%和1.2390。红外光谱图显示取代位置为N,O取代;13C-NMR谱图显示羧甲基几丁质是以6位上的一级取代为主,各位置的取代大小依次为6位羟基、-NH2和3位羟基。凝胶色谱结合多角激光光散射仪测定结果显示羧甲基几丁质的重均相对分子质量和数均相对分子质量及其分布系数分别为6.25×105、5.60×105和1.22。生物学性能检测结果显示羧甲基几丁质是一种无菌、无热原、无急性全身毒性、无细胞毒性、无皮内刺激、无皮肤致敏反应、无遗传毒性的生物材料,植入人体后对组织无毒副作用。结论通过碱化和醚化反应从几丁质中制备的羧甲基几丁质是一种脱乙酰度较低、取代度高、生物相容性良好的高分子生物医用材料。更多还原

【Abstract】 Objective To prepare carboxymethylchitin and study its properties. Methods Chitin was prepared from fresh shrimp shells and then carboxymethylchitin was prepared by the methods of alkalization and etherification as well as by the purification technique. The deacetylation degree of carboxymethylchitin was determined by the double-jump potentiometric titration method; the substitution degree was determined by the element analysis method; the carboxymethyl substitution position was analyzed by the Fourier transform infrared spectroscopy apparatus and the nuclear magnetic resonance spectroscopy apparatus; the relative molecular weight and its polydispersity were determined by the gel permeation chromatography with the multiple angle laser light scattering detection; the biological properties were tested according to the GB/T 16886 biological evaluation on medical devices. Results Carboxymethylchitin could be prepared by alkalization and etherification from chitin which was prepared from fresh shrimp shells by decalcification and deproteinization. The deacetylation degree of carboxymethylchitin was 13.76% according to the double-jump potentiometric titration; the degrees of deacetylation and substitution were 14.53% and 1.239 0 respectively according to the element analysis. The IR spectrum showed that the substitutive position was N, O-substitution, and the 13C-NMR spectrum showed that substitutive position of carboxymethylchitin was mostly primary substitution of 6-OH, and according to the substitutive proportion, the substitutive turns were in the following decreasing order: 6-OH, NH2, and 3-OH. The weight-averaged and the number-averaged molecular weights and polydispersity were 6.25×105, 5.60×105 and 1.22, respectively. The results from the biological property test showed that carboxymethylchitin was a biomaterial that was sterile, pyrogen-free, acute toxicity-free, cytotoxicity-free, intracutaneous irritation-free, skin sensitization-free and biomaterial genotoxicity-free, with no side or adverse effects on the related tissues after implantation into the human body. Conclusion Carboxymethylchitin prepared from chitin by alkalization and etherification is a macromolecule biomaterial that has a low degree of deacetylation, a high degree of substitution, and a good biocompatibility.更多还原