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将冰川棘豆阴干 ,粉碎 ,过 2 0目筛。用 15倍量MeOH冷渗 ,减压回收溶剂 ,浓缩物加 0 1mol/LHCl溶解 ,过夜 ,过滤 ,酸水液以 80 0～ 10 0 0ml/ (min·cm2 )流经H+ 阳离子交换树脂。树脂出柱 ,水洗去悬浮物 ,上柱继续洗至无色 ,改用Me2 CO洗至流出液遇NH3 ·H2 O不变色后 ,将树脂倒入烧杯中 ,加 2mol/LNH3 ·H2 O适量 ,密闭 30min ,挥去NH3 ·H2 O ,再上柱 ,Me2 CO洗脱 ,回收溶剂得粗提物 ,粗提物用 1%HCl溶解 ,CHCl3 振摇洗涤数次 ,酸水层调pH 10 ,CHCl3 萃取 ,减压回收溶剂得粗碱 ,用石油醚溶出总碱 ,经硅胶G(含微量NaOH)柱层析 ,CHCl3 Me2 CO恒沸物洗脱 ,每 10ml收 1份 ,TLC检查 ,同类合并 ,石油醚重结晶 ,得晶Ⅰ和晶Ⅱ。并对它们的理化特性进行了初步测定。
The glacial Oxytropis dried, crushed, over 20 mesh sieve. The solution was cooled under reduced pressure with 15 times the amount of MeOH and the solvent was recovered under reduced pressure. The concentrate was dissolved in 0 1 mol / L HCl, and the mixture was filtered overnight. The aqueous acid solution was flowed through the H + cation exchange resin at 80 to 10 0 ml / (min · cm2). Resin out of the column, washed with water to the suspended solids, the column continued to wash to colorless, use Me2 CO wash until the effluent met NH3 · H2 O does not change color, the resin into the beaker, add 2mol / LNH3 · H2 O amount, Airtight 30min, swirling NH3 · H2 O, and then on the column, Me2 CO elution, the solvent was recovered crude extract, crude extract was dissolved with 1% HCl, CHCl3 shake washed several times, the acid layer was adjusted to pH 10, CHCl3 Extraction, the solvent was recovered under reduced pressure to give a crude base, eluting the total base with petroleum ether, eluting with CHCl3 Me2 CO azeotrope on silica gel G (containing trace NaOH), collecting 1 part per 10 ml, checking by TLC, Petroleum ether recrystallization, crystal Ⅰ and crystal Ⅱ. And their physical and chemical properties of a preliminary determination.