甘肃棘豆化学成分研究 Ⅰ.碱水氯仿提取部位成分分析

Study on chemical component of oxytropis kansuensis Bunge.Ⅰ. Analysis of component in extractive position of alkalized chloroform

将甘肃棘豆草粉用甲醇浸提 ,浓缩浸提液后 ,1mol/l的盐酸酸解 ,抽滤 ,所得酸水液首先用氯仿萃取 8次后 ,然后用NaOH碱化 ,最后碱水液经氯仿萃取 4次后所得氯仿液减压浓缩即得碱水氯仿提取部位。取碱水氯仿提取部位 2 2 6g ,在氯仿 -乙酸乙酯 -甲醇洗脱体系下 ,柱层析梯度洗脱进行分离 ,每 3 0ml收集 1份 ,共收集 72 1份 ,TLC检测 ,合并同类 ,得晶体Ⅰ ,对晶体Ⅰ进行了分光光度和TLC鉴定。对碱水氯仿提取部位进行气质联用分析 ,共有 2 0种成分 ,确定了结构的成分有 10种 ,分别是生物碱 1种、酯 6种、醇 1种、芳香烃 1种、脂肪酸 1种 ,其它

Oxytropis kansuensis Bunge. powder was dripped in methanol, the residue following evaporated of the methanol was dissolved in 1 mol/l HCl and filtered. The acidified filtrate at first extracted 8 times by chloroform, second alkalized by NaOH, at last extracted 4 times by chloroform to obtain position of alkalized chloroform. Applied 22.6 g position of alkalized chloroform to a silica gel column and gradient eluted under system of chloroform-ethyl acetate-methanol, collected 30mL/fraction. 721 fractions was collected and monitored by TLC. Incorporated the same fraction to gain the crystalⅠwhich was identified by TLC and spectrophotometry. Analysed the position of alkalized chloroform with GC-MS to find 20 components, in which the structure of 1 alkaloid, 6 esters, 1 alcohol, 1 aromatic hydrocarbon, and 1 fatty acid were defined.