救必应药材经粉碎过筛后用50%乙醇超声提取,再以大孔吸附树脂XDA-1分离富集获得紫丁香苷粗提物,然后用制备型高效液相色谱法：采用Welchrom C18（4.6 mm×250 mm,10μm）色谱柱,优化条件,获得DACHB50（50 mm×1000 mm）制备色谱柱初始色谱条件;再以Chromatorex C18（10μm,300 g）为制备色谱柱填料,优化条件探索最佳进样量,并制备获得目标化合物。通过薄层色谱法和分析型高效液相色谱法对该化合物进行定性和定量分析,结果表明所得化合物的纯度为98.6%。以X-单晶衍射方法测定该化合物的分子结构信息,并解析数据,进一步确定该化合物是紫丁香苷。
In this study, Rex rotunda Thunb sample was pulverized and extracted with 50% ethanol. Consequently, the crude product of syringin was obtained from the ethanol crude extract through purification with XDA-l-macroporous adsorption resin. In order to prepare syringin with the preparative HPLC, the initial chromatographic conditions of the preparative DAC-HB50 column （50 mm × 1 000 mm;the packing material：chromatorex C18 ,10 μm,300 g） were investigated with the analytical welchrom C18 chromatographic column （4.6 mm × 250 mm, 10 μm） on the preparative HPLC. Furthermore,syringin was acquired from the crude product of syringin under the best loading amount that was sought through the optimization of the initial separation condition. Finally,the TLC and analytical HPLC analysis results showed that the final obtained product was syringin with the purity of 98.6%. The molecular structure was determined by single-crystal X-ray diffraction analysis. According to the data, the final obtained product was further confirmed as syringin.
Natural Product Research and Development
preparative high performance liquid chromatography
Ilex rotunda Thunb
single-crystal X-ray diffraction