海洋硫酸鼠李寡糖的制备研究

Research on the preparation of marine sulfated rhamno-oligosaccharides

目的探究海洋硫酸鼠李寡糖的制备方法并对所得寡糖的特征进行研究。方法采用三氟乙酸(TFA)和盐酸(HCl)对海洋硫酸鼠李多糖进行降解,通过薄层色谱法和凝胶渗透色谱法对降解条件进行分析,确定寡糖的制备方法;制备得到一系列硫酸鼠李寡糖,采用质谱法对其特征进行研究。结果 0.1mol·L^(-1) TFA、80℃及0.1mol·L^(-1) HCl、80℃水解条件对多糖的降解作用较好,且通过Bio-Gel P4凝胶色谱柱对寡糖能进行有效分离;最终选取0.1mol·L^(-1) HCl、80℃、10h的水解条件对硫酸鼠李多糖进行降解,采用Bio-Gel P4凝胶色谱柱对寡糖混合物进行分离纯化,负离子模式下的电喷雾质谱分析表明,这些寡糖为聚合度为1~11的硫酸化鼠李寡糖。结论首次建立了海洋新型硫酸鼠李寡糖的制备方法,这些硫酸鼠李寡糖为新型海洋特征寡糖。

Objective To explore the preparation methods of marine sulfated rhamno-oligosaccharides and their structural characteristics.Methods Degradation of the sulfated rhamnan was carried out by using trifluoroacetic acid（TFA）and hydrochloric acid（HCl）.The degradation products were analyzed by thin layer chromatography（TLC）and gel permeation chromatography.A series of sulfated rhamno-oligosaccharides were obtained and their characteristics were studied by negative-ion electrospray mass spectrometry（ES-MS）.Results The conditions ＂0.1 mol L-1 TFA 80℃＂ and ＂0.1 mol·L^（-1） HCl 80℃＂ had good effects on the degradation of the polysaccharide.The oligosaccharides could be effectively separated by Bio-Gel P4 gel chromatography.The condition ＂0.1 mol·L^（-1） HCl 80℃10 h＂ was finally chosen to degrade the sulfated rhamnan and the degradation product was further purified by Bio-Gel P4 gel chromatography.Negative-ion ES-MS analysis indicated that the oligosaccharides were rhamno-oligosaccharides with the degree of polymerization as 1~11.Conclusion The preparation method of the novel marine sulfated rhamno-oligosaccharides was established for the first time and the rhamno-oligosaccharides were novel marine oligosaccharides.