非均相磺化反应体系制备(1→3)-β-D-葡聚糖硫酸酯

Preparation of(1→3)-β-D-glucan sulfate employing a heterogeneous sulfation system

考察硫酸和正丙醇组成的非均相磺化反应体系制备(1→3)β--D-葡聚糖硫酸酯的可行性,利用元素分析、红外光谱、1H NMR、扫描电镜等技术对产物进行结构表征。结果表明,制备得到的(1→3β)--D-葡聚糖硫酸酯完全溶于水,质量收率约37.4%,经验式为(C6H10O5)25.9SO3.7H2O,红外谱图在1 240 cm-1、810 cm-1存在特征吸收带,1H NMR分析也支持产物为(1→3)-β-D-葡聚糖硫酸酯。

A novel glucan sulfation by a heterogeneous reaction system, composed of sulfuric acid and n-propanol with a molar ratio of 1.4, was proposed to improve polysaccharide polarity and its aqueous solubility. After the heterogeneous sulfation at -6 ℃ for 90 min, （1→3）-β-D-glucan sulfate mass yield was about 37.4%, and its empirical formula was （C6H10O5）25 · 9SO3 · 7H2O based on the results of elemental analysis. The presence of characteristic absorptions at 1 240 cm^-1 and 810 cm^-1 in the FTIR spectrum, as well as the ^1H NMR spectrum demonstrate that the material is a sulphate ester of glucan.