超声条件下蔗糖-6-月桂酸单酯及蔗糖-6’-月桂酸单酯的合成、纯化与结构鉴定

Synthesis,purification and identification of the 6-O-lauroylsucrose,6'-O-lauroylsucrose under ultrasonic condition

采用薄层层析(TLC)和硅胶柱层析分离纯化了超声处理条件下合成的蔗糖月桂酸单酯,并对纯化后的组分采用高效液相色谱(HPLC)、红外光谱(IR)、质谱(MS)、核磁共振(1H-NMR、13C-NMR)进行了结构鉴定和表征。TLC分离蔗糖月桂酸酯的理想条件:点样量4μL,以氯仿/甲醇/冰乙酸/水(V/V/V/V,75:15:7:3)展开25min,然后用10%磷钼酸乙醇溶液喷雾,105℃显色10min。硅胶柱层析分离蔗糖月桂酸酯的较佳条件为:3g样品溶于10mL洗脱剂上,35mm×700mm硅胶(200～300目)层析柱,流动相为TLC展开剂配比,流速为40～50mL/h,每30min收集一份洗脱液。两种单酯组分分别为蔗糖-6-月桂酸酯和蔗糖-6’-月桂酸酯。

The lauroylsucrose synthesis under ultrasonic condition were separated and purified by the thin layer chromatography（TLC） and silica gel column chromatography,and then the purified products were analyzed by HPLC,IR,MS and NMR. The optimum conditions for TLC were confirmed：4μL of the reaction mixture were applied to silica gel G plates, developed by chloroform-methanol-aceticacid-water（V/V/V/V, 75：15：7：3）, and then detected by spraying with 10% of phosphomolybdic acid hydrate in ethanol and heated at 105℃ for 10min. The optimum conditions for silica gel column chromatography were：3g sample dissolved in eluent was applied to 35mm×700mm silica gel column （200~300mesh） and chloroform-methanol-aceticacid-water was used as mobile phase,whose flow rate was 40~50mL/h,the eluent of 1 bottle/30min was collected. The purified products were 6-O-lauroylsucrose and 6＇-O-lauroylsucrose.