高纯度药用级蔗糖八硫酸酯钠的制备工艺研究

Study on Preparation Process of High Purity Pharmaceutical Grade Sucrose Octasulfate Sodium Salt

采用无水吡啶为催化剂可以有效地提高蔗糖八硫酸酯钠的产率及成品的纯度,探讨反应条件对结果的影响,得出最佳反应条件为:n(蔗糖):n(三氧化硫-吡啶复化物):n(催化剂)=1:6:11,保温时间为4 h,反应温度为80℃~90℃。采用醇-水重结晶的方法对粗产物进行提纯,重结晶两次后蔗糖八硫酸酯钠纯度可达99.8%,继续重结晶对纯度提高影响不大。同时开发了蔗糖八硫酸酯钠含量的检测方法。高纯度蔗糖八硫酸酯钠作为药用辅料满足高端药物制剂的需求。

The use of anhydrous pyridine as a catalyst can effectively improve the yield of sodium sucrose octasulfate and the purity of products. The effect of the reaction conditions on the synthesis was discussed, and the optimal reaction conditions were obtained: The molar ratio of sucrose, sulfur trioxide-pyridine compound and catalyst was 1:6:11, the holding time was 4 hour, and the reaction temperature was 80℃~90 ℃. The purification of crude products is carried out by the method of recrystallization of alcohol-water. After the second recrystallization, the purity of sodium sucrose octasulfate can reach about 99.8%, and continued recrystallization has little impact on the improvement of purity. At the same time, the detection method of sucrose octasulfate was developed. high-purity sucrose sodium octasulfate satisfies the application of pharmaceutical excipients in medicine.