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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 investigate the preparation of marine alginate rhamnose oligosaccharides and to study the characteristics of the resulting oligosaccharides. Methods Trifluoroacetic acid (TFA) and hydrochloric acid (HCl) were used to degrade the polysaccharides of R. solanacearum, and the degradation conditions were analyzed by TLC and gel permeation chromatography to determine the preparation method of oligosaccharides. A series of Rhamnose sulfate oligosaccharides, its characteristics were studied by mass spectrometry. Results The degradation of polysaccharides by 0.1 mol·L -1 TFA, 80 ° C and 0.1 mol·L -1 HCl at 80 ° C was better than that of the control by Bio-Gel P4 gel column Sugar can be effectively separated; the final selection of 0.1mol · L -1 HCl, 80 ℃, 10h hydrolyzing conditions on the degradation of rhamnose sulfate, the use of Bio-Gel P4 gel column oligosaccharide mixture was isolated and purified Electrospray ionization mass spectrometry analysis in negative ion mode showed that these oligosaccharides were sulfated rhamnose oligosaccharides with a degree of polymerization of 1-11. Conclusions A new marine preparation method for rhamnosyl sulfate was established for the first time. These rhamnose sulfates are novel marine-characterized oligosaccharides.