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Method for extracting silymarin from silybum marianum

A milk thistle and water extraction technology, which is applied in the field of separation and extraction of silymarin, can solve the problems of human harm, benzene is not suitable for industrial production, and benzene is highly toxic, and achieves the effect of convenient operation

Active Publication Date: 2015-06-17
三原润禾生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Patent CN101817816A The method for preparing silibinin uses benzene and ethyl acetate to elute, because benzene is highly toxic and harmful to the human body, and foreign countries have strict requirements on the residual amount of benzene in products, so benzene is not suitable for industrialization Production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) extract

[0044] Pulverize the milk thistle raw material to obtain a pulverized product, add 35% alumina of the raw material quality of the milk thistle to the pulverized product and mix, and extract the mixture with 4 times the amount of ethyl acetate of the raw material quality of the milk thistle, and the extraction temperature is 70°C to obtain the extract;

[0045] (2) Column chromatography

[0046] Put the obtained extract on column chromatography, the column chromatography filler is magnesium oxide, and the filler is twice the amount of the raw material quality of milk thistle, followed by petroleum ether: ethyl acetate (50:1), petroleum ether: ethyl acetate (20: 1), ethyl acetate: ethanol (20:1), ethyl acetate: ethanol (5:1) for gradient elution; TLC detection;

[0047] After the active ingredients are completely eluted by TLC, the eluents of each stage are concentrated, placed to crystallize, and suction filtered to obtain crude crystals of silybin, silyb...

Embodiment 2

[0052] (1) extract

[0053] The raw material of milk thistle is crushed to obtain a pulverized product, and 10% of the mass of the raw material of milk thistle is added to the pulverized product. Aluminum oxide is mixed, and the mixture is extracted with ethanol in an amount 3 times the mass of the raw material of milk thistle, and the extraction temperature is 50°C , to obtain the extract;

[0054] (2) Column chromatography

[0055] Put the obtained extract on column chromatography, the column chromatography filler is silica gel, and the filler is 0.5 times the quality of milk thistle raw material, followed by petroleum ether: ethyl acetate (20:1), petroleum ether: ethyl acetate (5:1 ), ethyl acetate: ethanol (5:1), ethyl acetate: ethanol (1:1) for gradient elution, TLC detection;

[0056] After the active ingredients are completely eluted by TLC, the eluents of each stage are concentrated, placed to crystallize, and suction filtered to obtain crude crystals of silybin, sil...

Embodiment 3

[0060] Embodiment three (best embodiment)

[0061] (1) extract

[0062] The milk thistle raw material is crushed to obtain a pulverized product, and 50% of the mass of the milk thistle raw material is added to the pulverized product to mix, and the mixture is extracted with ethyl acetate of 6 times the mass of the milk thistle raw material, and the extraction temperature is to 70°C to obtain the extract;

[0063] (2) Column chromatography

[0064] Put the obtained extract on column chromatography, the column chromatography filler is aluminum oxide, the filler is 1.5 times the amount of milk thistle raw material quality, followed by petroleum ether: ethyl acetate (28:1), petroleum ether: ethyl acetate (10:1) 1), ethyl acetate: ethanol (12:1), ethyl acetate: ethanol (3:1) for gradient elution; TLC detection;

[0065] After the active ingredients are completely eluted by TLC, the eluents of each stage are concentrated, placed to crystallize, and suction filtered to obtain crud...

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PUM

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Abstract

The invention provides a method for extracting silymarin from silybum marianum, which has the advantages of providing a convenient, rapid and stable process route, optimizing the extraction step, reducing the production cost and improving the operability. The technical thought of the invention is mainly embodied in the following steps of smashing raw materials, mixing and adding oil adsorbents, carrying out extraction by adopting an organic solvent, directly adsorbing the extracting solution which is not concentrated by utilizing column chromatography, carrying out gradient elution by adopting mixed solvents of petroleum ether and ethyl acetate as well as ethyl acetate and ethanol, carrying out thin-layer chromatographic detection, carrying out fractional collection, mixing the same effluent with the main ingredient eluent, concentrating, crystallizing and recrystallizing the effluent. With the adoption of the method, contents of the obtained isosilybin, silibinin, silydianin, silychristinin can be up to about 95% and recovery rates of effective ingredients are greater than 90%.

Description

technical field [0001] The present invention relates to a method for extracting silymarin, in particular to a method for separating and extracting silymarin (four products of silybin, silybin, silybinin and silymarin) from milk thistle seeds method. Background technique [0002] Milk thistle [Silybum marin (L.) Gaertn.], also known as Our Lady's thistle, milk fly, and milk thistle, is a herb of the genus Asteraceae. Native to Western Europe and North Africa, it is cultivated in Shaanxi, Gansu, Heilongjiang and Hebei provinces in China. The whole plant contains flavonoids and fumaric acid; the seeds contain silibinin, isosilibinin, dehydrosilibinin, silybinin, silybinin, silybin polymer and cinnamic acid, myristate Acid, palmitoleic acid, arachidic acid, etc. [0003] The main product of milk thistle is silymarin. Silymarin is a kind of flavonoid lignans extracted from the fruit and seeds of milk thistle and condensed with phenylpropanoid derivatives. Silymarin is its main...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D407/04
Inventor 王晓莹肖红王春德杨军仁
Owner 三原润禾生物科技有限公司