摘要
主要研究甘草查尔酮分离纯化工艺:①将甘草粉碎,用φ=95%的乙醇浸泡三次,合并其三次的提取液,浓缩回收溶剂后,得到甘草粗提物;将甘草粗提物用pH=9～10的石灰水热溶,除去鞣质和胶质,过滤,滤液用ω=5%Na2CO3溶液和乙酸乙酯反复萃取3～4次,回收酯溶液,得到含有查尔酮的稠膏.②稠膏用甲醇溶解,拌入聚酰胺,真空干燥成粉状物,用聚酰胺柱层析分离,用不同体积分数的乙醇做洗脱液,分段检验洗脱液,收集有查尔酮特征的洗脱液,浓缩后得到黄色固体查尔酮;用V(甲苯)∶V(氯仿)∶V(丙酮)=40∶25∶35混合溶剂进行硅胶柱层析,分段检验洗脱液,收集有查尔酮特征的洗脱液,浓缩回收混合溶剂,可得淡黄色晶体,再用甲醇重结晶,得到亮黄色针状结晶查尔酮.研究结果表明:采用柱层析分离纯化工艺可得到纯度较高的甘草查尔酮.
To develop the process of the separation and purification of Charles ketone in licorice, it was firstly smashed and extracted three times by ethanol solution. Then the ethanol solution from three times extractive operations was mixed and concentrated to remove solvent and obtain crude extract. The crude Charles ketone was dissolved into hot lime solution （pH9- 10） and filtered to remove tanning and cementing substance. The filtrate was extracted three or four times by the solution of 5% Na2CO3 and acetic ether. The recovered acetic ether solution contained thick Charles ketone extract. It was dissolved into methanol, which was evaporated as polyamide was added, and dried under vacuum. The powdered-product was found and dissolved into the water. This solution was introduced to polyamide chromatographic column and washed by a various of concen- trations of ethanol solution. The washing solution was tested in different section of column to collect the solution which showed the characteristics of Charles ketone. The obtained yellow solid Charles ketone was dissolved into a mixed solution of methylbenzene, chloroform and acetone （40： 25： 30） then introduced into silica gel chromatographic column. The solution, which contained Charles ketone in different section of column, was collected and concentrated. The recovered light yellow crystal was recrystallized in methanol solution. Finally, the bright yellow needle-like Charles ketone crystal was obtained. This research presented that the high purified Charles ketone could be obtained by the column chromatographic separation process. It is also the method of separation and purification of Charles ketone in laboratory.
出处
《宁夏工程技术》
CAS
2005年第4期363-365,共3页
Ningxia Engineering Technology
关键词
查尔酮
柱层析
分离
纯化
Charles ketone
column chromatograph
separation
purification
