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杜仲醇的提取分离及合成积累动态研究

Study on Extraction & Isolation and Dynamic Accumulating of Eucommiol

【作者】 彭金年

【导师】 苏印泉; 车庆明;

【作者基本信息】 西北农林科技大学 , 森林培育学, 2004, 硕士

【摘要】 将杜仲醇对照品配制成一定浓度的标准溶液系列,用高效液相色谱仪测定其含量,绘制标准曲线,确定了高效液相色谱法测定杜仲醇含量的色谱条件:色谱柱:ODS;流动相:甲醇∶水=10∶90;检测波长:210nm;流速:1mL/min。采用单因素和正交试验的方法,对影响杜仲醇提取率的主要因素进行了分析,并用高效液相色谱仪测定了不同提取条件下杜仲醇的含量,确定了杜仲醇的最佳提取条件:原材料粉碎,加10倍量蒸馏水在80℃水浴回流提取2次,每次2h。研究确定了杜仲醇的提取分离工艺:原料加10倍量蒸馏水在80℃水浴回流提取2次,每次2h。滤液合并、浓缩,以95%乙醇沉淀,醇液浓缩至一定浓度,反复上D-101大孔吸附树脂柱进行分离,水洗脱,TLC检测,CHCl3-MeOH-H2O(7:3:0.5) 展开,收集10%硫酸乙醇溶液显粉紫色的部分。富集一定量样品上硅胶柱分离,5%、10% CHCl3-MeOH溶液依次洗脱,收集10% CHCl3-MeOH洗脱部分,浓缩后得无色油状物,即杜仲醇。采用不同杀青方法对杜仲鲜叶进行处理,粉碎,加10倍量蒸馏水在80℃水浴回流提取2次,每次2h,用高效液相色谱仪测定杜仲醇含量。结果表明:用烘箱在100℃烘30min后,自然阴干处理的杜仲叶中杜仲醇含量最高,为有效提取杜仲醇的最佳预处理方法。对不同栽培模式、不同生长季节杜仲叶和杜仲皮中杜仲醇的含量进行测定,方差分析结果显示,不同栽培模式、不同生长季节杜仲叶和杜仲皮中杜仲醇含量均存在极显著差异。其合成积累动态规律如下:乔林栽培模式下的杜仲叶,杜仲醇含量在7月中旬出现第一个高峰,9月中旬达到第二个高峰,且为全年最高值,8-10月间含量保持较高水平;叶林栽培模式下的杜仲叶,杜仲醇含量在5-6月比较稳定,且为全年最高值,9月中旬达到第二个高峰;乔林栽培模式下的杜仲当年生枝皮,杜仲醇的含量只在6月中旬有一个高峰,且在5-6月呈比较稳定的增长趋势;叶林栽培模式下杜仲皮杜仲醇的含量春季明显高于秋季(约6倍)。对不同的栽培模式及药用部位而言,乔林叶中杜仲醇的含量较之叶林叶要高;而乔林皮中杜仲醇的含量较之叶林皮要低。

【Abstract】 The standard eucommiol sample was mixed with H2O to form a certain concentration solution series. The content of eucommiol was measured by HPLC and the chromatographic conditions were determined. The chromatogram column was ODS, the elution was MeOH- H2O (10:90), the detect wave was 210 nm and the velocity of flow was 1ml/min.The main factors influenced the extract rate of eucommiol were anaysized. The best extract conditions were determined. The materials shattered and were supplied with 10 times water. This mix was heated 2 hours at 80℃ and filtered. The process was repeated again.The technics of extraction and isolation of eucommiol was determined. The extract was condensed then subsided by ethanol. The solution was condensed, then eluted with H2O through the D-101 resin repeatedly. At the same time the elutions were detected by TLC, and spreaded by CHCl3-MeOH-H2O (7:3:0.5). The part presented mauve against 10% H2SO4-CH3CH2OH was gathered, then condensed and subjected to the silica gel column eluting with 5% and 10% CHCl3-MeOH in turn. The section eluted with 10% CHCl3-MeOH was gathered and condensed, that is eucommiol.Comparing the effect of different treatments with Eucommia leaves on the content of eucommiol, we found that the content of eucommiol is highest by the treatment with toasted 30 minutes at 100℃ then cooled naturally.Analyzing the content of eucommoil in Eucommia leaves and Eucommia cortex from different models in different seasons shows that in different models and different seasons the content of eucommoil is different. Speaking of the tree model, the content of eucommoil in leaves reached its first maximum in July, and then reached its second maximum in September, which was the highest of the whole year. From August to October the content of eucommoil was at the stable and high standard. The content of eucommoil in cortex reached its maximum in June, and increased stably in the following two months.. While as to the leaf model, the content of eucommoil in leaves was stable and highest in May and June, then reached its second maximum in September. The content of eucommoil in cortex was higher in spring than in autumn.

  • 【分类号】TQ28
  • 【被引频次】7
  • 【下载频次】437
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