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Separation and purification method for ingenol monomers

A technology for the separation and purification of ingenol, which is applied in the field of separation and purification of ingenol monomers and the preparation of plant compound monomers, can solve the problems of no production and extraction process, and achieve product quality, product quality control, and energy saving The effect of production costs

Active Publication Date: 2014-04-02
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are fewer reports on the research on ingenol monomer in Stephania chinensis, and there is no more mature production and extraction process.

Method used

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  • Separation and purification method for ingenol monomers
  • Separation and purification method for ingenol monomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 1) extract

[0041] Grind 20 kg of Stephania chinensis into a coarse powder of 1-4 mm, add 160 L of ethanol solution with a concentration of 90% by volume, extract 3 times, each time for 2 hours, recover ethanol, and combine the filtrate, a total of 6000 ml;

[0042] 2) extraction

[0043] The filtrate obtained in step 1) was added with an equal volume of ethyl acetate to extract 3 times, and the upper layer solution was separated and concentrated to dryness to obtain a concentrated solution of 3000 ml, which was then processed in the next step;

[0044] 3) Silica gel column chromatography

[0045] Add the concentrated solution obtained in step 2) to 10 times the weight of silica gel to mix the sample, dry the mixed silica gel at 50°C, elute the product with petroleum ether: ethyl acetate (1:1 volume ratio), and concentrate the column chromatography product solution at 50°C to Dry to obtain 1.0 g of solids;

[0046] 4) Dissolving and filtering

[0047] Add 40ml of m...

Embodiment 2

[0060] 1) extract

[0061] Grind 60 kg of Stephania chinensis medicinal material into a coarse powder of 1-4 mm, add 360 L of ethanol solution with a concentration of 95% by volume, extract 4 times, each time for 3 hours, recover ethanol, and combine the filtrate, a total of 15000 ml;

[0062] 2) extraction

[0063] The filtrate obtained in step 1) was extracted by adding an equal volume of ethyl acetate for 3 times, and the upper layer solution was separated and concentrated to dryness to obtain 5000 ml of concentrated solution, which was then processed in the next step;

[0064] 3) Silica gel column chromatography

[0065] Add the concentrated solution obtained in step 2) to 10 times the weight of silica gel to mix the sample, dry the mixed silica gel at 50°C, elute the product with petroleum ether: ethyl acetate (1:1 volume ratio), and concentrate the column chromatography product solution at 50°C to Dry to get 4.0 grams of solids;

[0066] 4) Dissolving and filtering

...

Embodiment 3

[0080] 1) extract

[0081] Grind 20 kg of Stephania chinensis into a coarse powder of 1-4 mm, add 160 L of ethanol solution with a concentration of 95% by volume, extract 3 times, each time for 2 hours, recover ethanol, and combine the filtrate, a total of 5000 ml;

[0082] 2) extraction

[0083] The filtrate obtained in step 1) was added with an equal volume of ethyl acetate to extract 3 times, and the upper layer solution was separated and concentrated to dryness to obtain 2000ml of concentrated solution, which was then processed in the next step;

[0084] 3) Silica gel column chromatography

[0085] Add the concentrated solution obtained in step 2) to 10 times the weight of silica gel to mix the sample, dry the mixed silica gel at 50°C, elute the product with petroleum ether: ethyl acetate (1:1 volume ratio), and concentrate the column chromatography product solution at 50°C to Dry to get 1.2 grams of solids;

[0086] 4) Dissolving and filtering

[0087] Step 3) Add 40m...

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Abstract

The invention relates to a separation and purification method for ingenol monomers, and belongs to the technical field of the separation and purification for the active ingredients of traditional Chinese medicines. The separation and purification method disclosed by the invention comprises the following steps: by taking the traditional Chinese medicine moleplant seeds of euphorbia as raw materials, performing ethanol solution extraction, ethyl acetate extraction, silica-gel column chromatography, methanol dissolution and filtration, preparative high-performance liquid chromatographic separation and product recovery to obtain ingenol monomer products. According to the separation and purification method disclosed by the invention, the content of ingenol in the products achieves more than 98% by virtue of the optimum process and parameter conditions; the whole technical process is stable, simple and convenient to operate, high in separation efficiency, and low in cost, and is capable of separating and preparing the ingenol monomers with a high purity.

Description

technical field [0001] The invention relates to a preparation method of a plant compound monomer, in particular to a separation and purification method for extracting ingenol monomer from Stephania chinensis, belonging to the technical field of separation and purification of traditional Chinese medicines. Background technique [0002] Qianjinzi is the seed of Euphorbialathyris L., a plant of Euphorbiaceae. Also known as Qianliang Gold, Bodhisattva Dou ("Rihuazi"), Xu Suizi ("Kaibao Materia Medica"), Judongshi ("Bencao Tujing"), Lianbu ("Doumen Fang"), Judongzi ( "Compendium of Materia Medica"), Tanbanjiu ("Hunan Drug Records"), Kanyuanlao ("Guizhou Herbal Medicine"), Baiyaojie, Ganjinyaojie ("Yunnan Medicinal Plants"), Xiaocrodou ("Guizhou Herbal Medicine") Shanxi Chinese Herbal Medicine"). The original plant Suizi is also known as: Resisting Winter ("Kaibao Materia Medica"), Banzhilian ("Compendium Supplements"), Jianglongcao ("Shaanxi Traditional Chinese Medicine List")....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/727C07C45/78C07C45/80C07C45/79
CPCC07C45/78C07C2603/86C07C49/727
Inventor 陈冲文焕松夏柯刘丁
Owner CHENGDU PUSH BIOLOGICAL TECH
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