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The preparation method of 5-methylmelissain

A technology of methyl honey and aspergillus, applied in directions such as organic chemistry, can solve problems such as no research report, and achieve the effects of simple process, high purity and low production cost

Active Publication Date: 2015-09-16
ZHEJIANG JOLLY PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to the results of literature search, there is no research report in this area

Method used

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  • The preparation method of 5-methylmelissain
  • The preparation method of 5-methylmelissain

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 100 g of Wuling bacteria powder, put it in a reflux bottle, add 6 times the amount of organic solvent (methanol, ethanol, n-butanol, ethyl acetate), heat and reflux for extraction for 1 hour, extract twice, filter, combine the filtrates, and decompress the filtrates Concentrate to about one-ninth of original volume. Put the concentrated solution in an extraction funnel and mix it with petroleum ether 1:1-5, shake and extract 5 times, combine the petroleum ether layer, concentrate under reduced pressure to a thick paste, and add about 600ml of ethanol to dissolve. Column chromatography silica gel (200-300 mesh) was used as the stationary phase, ethanol was used as the mobile phase, and the flow rate was 0.5 times the bed volume / hour to elute, and the eluate of the green fluorescent part was collected. The eluate was concentrated under reduced pressure, evaporated to dryness, heated to dissolve with a small amount of petroleum ether, allowed to cool, placed in a refr...

Embodiment 2

[0026] Take 100g of Wuling bacteria powder, put it in a reflux bottle, add 8 times the amount of organic solvent (methanol, ethanol, n-butanol, ethyl acetate), heat and reflux for extraction for 1 hour, extract twice, filter, combine the filtrates, and concentrate the filtrates under reduced pressure to about one-ninth of the original volume. Put the concentrated solution in an extraction funnel and mix it with petroleum ether 1:1-5, shake and extract 5 times, combine the petroleum ether layer, concentrate under reduced pressure to a thick paste, and add about 600ml of ethanol to dissolve. Column chromatography silica gel (200-300 mesh) was used as the stationary phase, ethanol was used as the mobile phase, and the flow rate was 1 times the bed volume / hour to elute, and the eluate of the green fluorescent part was collected. The eluate was concentrated under reduced pressure, evaporated to dryness, heated to dissolve with a small amount of petroleum ether, allowed to cool, pla...

Embodiment 3

[0028] Take 100g of Wuling bacteria powder, put it in a reflux bottle, add 10 times the amount of organic solvent (methanol, ethanol, n-butanol, ethyl acetate), heat and reflux for extraction for 1 hour, extract twice, filter, combine the filtrates, and decompress the filtrates Concentrate to about one-ninth of original volume. Put the concentrated solution in an extraction funnel and mix it with petroleum ether 1:1-5, shake and extract 5 times, combine the petroleum ether layer, concentrate under reduced pressure to a thick paste, and add about 600ml of ethanol to dissolve. Column chromatography silica gel (200-300 mesh) was used as the stationary phase, ethanol was used as the mobile phase, and the flow rate was 1.5 times the bed volume / hour for elution, and the eluate of the green fluorescent part was collected. The eluate was concentrated under reduced pressure, evaporated to dryness, heated to dissolve with a small amount of petroleum ether, allowed to cool, placed in a r...

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Abstract

The invention relates to an extraction and separation method for effective components of traditional Chinese medicines, and especially relates to a preparation method for an effective component extracted and separated from wuling mycelia powder. The invention relates to a preparation method for 5-methylmellein. The preparation method comprises steps of 1) digestion and condensation, 2) extraction and condensation, 3) chromatographic separation and 4) recrystallization. According to the preparation method, an one-step adsorption-desorption method is formed, the technology is simple, and the 5-methylmellein with high purity, a white crystal compound, is prepared. The product has advantages of high content of effective components, stable quality, good color, low production cost, high purity, small loss and high product quality.

Description

technical field [0001] The invention relates to a method for extracting and separating active ingredients of traditional Chinese medicines, in particular to a method for preparing active ingredient compounds extracted and separated from Wuling bacteria powder. Background technique [0002] The extraction and separation of active components of traditional Chinese medicine is a key step in realizing the modernization of traditional Chinese medicine. How to complete the extraction and separation of active components of traditional Chinese medicine on the basis of respecting the tradition of traditional Chinese medicine has always been a problem that has plagued the majority of Chinese medicine workers. Wuling bacteria powder is a national first-class new drug obtained by Zhejiang Zuoli Pharmaceutical Co., Ltd. by using modern biological fermentation technology to separate the bacteria from natural Wuling ginseng. The chemical composition mainly contains adenosine-based nucleosid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/76
Inventor 陈建逯振宇李福朱方剑林丽萍姚瑶秦序锋潘旖泮灿辉
Owner ZHEJIANG JOLLY PHARMA
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