冰川棘豆生物碱分析及苦马豆素的分离、鉴定  

Detection of Alkaloid and Isolation of Swainsonine from Oxytropis glacialis

作　　者：李勤凡[1] 王建华[1] 李蓉[1] 陈亚[1] 刘志滨[1] 

机构地区：[1]西北农林科技大学动物科技学院,杨凌712100

出　　处：《畜牧兽医学报》2005年第12期1339-1343,共5页ACTA VETERINARIA ET ZOOTECHNICA SINICA

基　　金：国家自然科学基金项目(30070577);西北农林科技大学科研专项基金(080807)

摘　　要：冰川棘豆干粉,经甲醇提取,盐酸酸化,酸水液用氯仿萃取数次,NaOH调pH至9～10,依次用氯仿、乙酸乙酯、正丁醇萃取.称重表明生物碱多集中在正丁醇组分,且以大极性生物碱为主.薄层层析检查结果显示,氯仿组分有10种生物碱,乙酸乙酯组分有7种生物碱,正丁醇组分有5种生物碱.将正丁醇组分经硅胶柱层析,乙酸乙酯一甲醇系统梯度洗脱,每30～50 mL收集1份,薄层层析监测,同类合并.Ehrlich's试剂显色明显段油浴升华,得到白色针状结晶,与苦马豆素标准样品进行薄层层析对照,其斑点形状、颜色相同,Rf值相近.通过熔点和IR、MS、1HNMR、13CNMR等鉴定其化学结构,为苦马豆素.The residue was extracted by hot methanol from Oxytropis glacialis powder, acidified with 1mol/L HC1 and filtrated to get acid liquid The acid liquid was extracted with chloroform to remove impurity. Then, its pH was adjusted to 9-10 with NaOH. The solution was extracted respectively with chloroform,ethyl acetate and n-butanol. The most alkaloids were maximum polarity in the butanol phase, with TLC checking on alkaloid,there were 10 alkaloids in chloroform phase, 7 alkaloids in ethyl acetate and 5 alkaloids in butanol phase. Applied the crude alkaloid extracted with butanol to a silica gel column, eluted with different proportion of ethyl acetate and methanol, collected 30-50 mL as one sample, monitored by TLC, incorporated the same fraction. The Ehrlich＇s colorable fraction were sublimated and white needles crystal were obtained The crystal was detected by TLC, which appeared the same dot shape, color and Rf as the standard swainsonine. The results preliminary determined that crystal was swainsonine. The chemical structures were identified as swainsonine by means of MP and IR, MS, ^1HNMR, ^13CNMR.

关 键 词：冰川棘豆 生物碱 苦马豆素 鉴定 

分 类 号：S859.87[农业科学—临床兽医学]