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Production method of high-purity silibinin

A technology of silibinin and production method, which is applied in the production field of high-purity silibinin, can solve the problems of harmful and toxic organic solvent residues, high impurity content, environmental pollution, etc., achieve solvent saving, safe operation, and reduce pollution Effect

Inactive Publication Date: 2013-11-27
天津普拉德生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to solve the technical problems of harmful and toxic organic solvent residues in the existing silibinin extraction and preparation process, pollute the environment, low yield and high impurity content, and provide a simple, efficient, no harmful and toxic solvent residue, product Production method of high-purity silibinin with high purity, environmental friendliness and suitable for technological production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 500 kg of milk thistle seeds were dehulled and separated from the seed coat by a sheller to obtain 250 kg of milk thistle seed coat, and 750 L of ethanol with a volume concentration of 60% was added, and 70 o Stir and extract at ℃ for 3 h, drain, then add 500 L of 60% ethanol to the extraction kettle,

[0038] 70 o Stir and extract at C for 2 h, release the liquid, combine the two extracts, concentrate under reduced pressure to recover ethanol, add water to dilute to 1000 L, let stand for 12 h, and filter to obtain the clear liquid.

[0039] Put 400 L of MG-1 gel-type hydrogen bond adsorption resin (Tianjin Ou Rui Biotechnology Co., Ltd.) on the clear night, control the flow rate of 200 L / h, wash 600 L with 15% ethanol after the adsorption, and flow rate of 300 L / h.

[0040] After rinsing, use 2000 L of ethanol with a volume concentration of 85% for desorption at a flow rate of 400 L / h, collect the effluent and rinse solution, and concentrate under reduced pressure to ...

Embodiment 2

[0044] 250 kg of milk thistle seeds were dehulled and separated from the seed coat by a sheller to obtain 125 kg of milk thistle seed coat, and 500 L of ethanol with a volume concentration of 75% was added, and 85 o Stir and extract at C for 3 h, discharge the liquid, then add 500 L of 75% ethanol to the extraction kettle, 85 o Stir and extract at C for 2 h, release the liquid, combine the two extracts, concentrate under reduced pressure to recover ethanol, add water to dilute to 750 L, let stand for 12 h, and filter to obtain the clear liquid.

[0045] 200 L of MG-2 gel-type hydrogen bond adsorption resin (Tianjin Orui Biological Technology Co., Ltd.) was applied in the clear night, and the flow rate was controlled at 100 L / h. After the adsorption was completed, 300 L was washed with 10% ethanol at a flow rate of 150 L / h.

[0046] After washing, desorb with 600 L of ethanol with a volume concentration of 75% at a flow rate of 150 L / h, collect the effluent and rinse solution, ...

Embodiment 3

[0050] 100 kg of milk thistle seeds were dehulled and separated from the seed coat by a sheller to obtain 54 kg of milk thistle seed coat, and 270 L of ethanol with a volume concentration of 90% was added, and 50 o Stir and extract at C for 3 h, drain the liquid, then add 270 L of 90% ethanol to the extraction kettle, 50 o Stir and extract at C for 2 h, release the liquid, combine the two extracts, concentrate under reduced pressure to recover ethanol, add water to dilute to 110 L, let stand for 12 h, and filter to obtain the clear liquid.

[0051] 100 L of OU-1 gel-type hydrogen bond adsorption resin (Tianjin Ou Rui Biotechnology Co., Ltd.) was applied in the clear night, and the flow rate was controlled at 50 L / h. After the adsorption was completed, 120 L was washed with 5% ethanol at a flow rate of 60 L / h.

[0052] After washing, desorb with 200 L of ethanol with a volume concentration of 60% at a flow rate of 60 L / h, collect the effluent and rinse solution, and concentrate...

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PUM

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Abstract

The invention provides a production method of high-purity silibinin. Silybum marianum seed is used as a raw material according to the method. The method comprises the steps of husking silybum marianum seeds, extracting by using an organic solvent aqueous solution, carrying out reduced-pressure concentration for recovering the solvent, diluting with water, removing precipitate, absorbing by using gel-type hydrogen bond adsorbent resin, washing for removing impurities, desorbing through a high-concentration organic solvent aqueous solution, decolorizing the desorption solution, concentrating and crystallizing the solution, recrystallizing and drying the solution to obtain a high-purity silibinin product, wherein the content of silibinin is more than 95%. The product is applicable to development of healthcare products, functional food and medicines. The method has the advantages that the product has high purity and stable quality and is free of residue of toxic and harmful solvent; the process is simple, convenient and rapid, and production cost is low; no toxic organic solvent is used in the processes; the production process is safe and environment-friendly.

Description

technical field [0001] The invention relates to a production method of high-purity silybin, and belongs to the technical field of extraction and separation of natural plant active ingredients. Background technique [0002] Silymarin (silymarin) is a mixture of flavonoid lignans. It is a natural active substance extracted from the seeds of the Compositae plant Silybum marianum. Its main components are silybin, isosilibin, silymarin There are 7 isomers including Jiting and Silyjining. Silibinin is a mixture of two diastereomers, silibinin A and silibinin B, in equal amounts. It is the main active ingredient of silymarin, accounting for about 60-70% of silymarin. Silybin can protect the liver by stabilizing the liver cell membrane, improving liver function, promoting liver cell membrane repair and regeneration, anti-hepatic fibrosis, anti-oxidation, anti-inflammation, immune regulation, etc. It is used in China, Germany, Japan and other countries It is clinically used to tre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D407/04
Inventor 欧来良漆敏王为超
Owner 天津普拉德生物科技有限公司
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