氨基磺酸法制备硫酸酯化十二指肠糖肽

Preparation of sulfated duodenum glycopeptide by sulfamic acid

为建立一种环保、经济且条件易控制的十二指肠糖肽硫酸酯化方法,以产物硫含量为评价指标,将甲酰胺作为溶剂,对比了氨基磺酸和氯磺酸2种磺化剂的效果。在对反应时间、温度、磺化剂和糖肽比例、溶剂和糖肽比例进行单因素影响分析的基础上,对氨基磺酸-甲酰胺法进行了正交试验,产物最高硫含量达20.5%,最佳工艺条件为糖肽质量和甲酰胺体积之比1∶7、糖肽质量和氨基磺酸质量比1∶5、温度80℃、时间7 h。以迁移率为指标对酯化产物进行了琼脂糖电泳分析,结果显示酯化产物分子量增加约6.0×103,红外光谱分析证明糖肽分子上连入硫酸酯基。

This study was to establish an environment friendly,low-cost,manageable method of sulfating duodenum glycopeptide.The effects of two esterifying agents of sulfamic acid and chlorosulfonic acid were compared with the sulfur content of the product,as the evaluation index,and formamide was the solvent.Based on the single factor experiment of reaction time,temperature,ratio of sulfonating agent and glycopeptide,ratio of solvent to glycopeptide,orthogonal experiment was carried out for aminosulfonic acid method.The optimum conditions were as follows： temperature 80 ℃,time 7 h,the ratio of glycopeptide mass to formamide volume 1 ∶ 7,and themass ratio of glycopeptide to sulfamate 1 ∶ 5. The sulfur content was 20. 5%. The agarose gel electrophoresis of the esterified product was carried out with mobility of different samples as an index,it was indicated that the molecular weight of esterified product increased about 6. 0×10^3,confirming that the sulfate group was linked to the polysaccharide molecule.