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Method for preparing Silymarin

A technology of silymarin and silymarin, which is applied in the field of silymarin preparation, and can solve the problems of serious pollution, unfavorable large-scale production operations, and low silymarin content

Inactive Publication Date: 2010-06-30
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the prior art, the extraction and separation method of silymarin mainly adopts organic solvent method, etc., but the content of silymarin obtained by these extraction processes is low, the pollution in the production process is serious, and it is unfavorable for large-scale production operations

Method used

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  • Method for preparing Silymarin

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Experimental program
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Effect test

Embodiment 1

[0018] Get milk thistle fruit fine powder (60 orders of particle size) 10Kg, join in CO 2 In the supercritical extractor, methanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 2%, the extraction pressure is 10MPa, the temperature is 30°C, and CO 2 The flow rate is 1ml / g crude drug / min, the extraction time is 150min, the extract is obtained, add acetone, stir to dissolve, filter, take the filtrate, concentrate, pour into a high-efficiency countercurrent extractor, and use water-acetone-chloroform (1:5:2) Solvent system, the lower phase is the stationary phase, the upper phase is the mobile phase, collect the silymarin segment, concentrate, precipitate crystals, separate the crystals, add acetone-petroleum ether (0.5:1) for recrystallization, separate, wash, and dry to obtain 9.1 g of silymarin , detected by HPLC, the purity was 91.2%.

Embodiment 2

[0020] Get milk thistle fruit fine powder (60 orders of particle size) 10Kg, join in CO 2 In the supercritical extractor, methanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 6%, the extraction pressure is 40MPa, the temperature is 60°C, and the CO 2 The flow rate is 5ml / g crude drug / min, the extraction time is 250min, the extract is obtained, add acetone, stir to dissolve, filter, take the filtrate, concentrate, inject high-efficiency countercurrent extractor, and use water-acetone-chloroform (1:5:2) Solvent system, the lower phase is the stationary phase, the upper phase is the mobile phase, collect the silymarin segment, concentrate, precipitate crystals, separate the crystals, add acetone-petroleum ether (2:1) for recrystallization, separate, wash, and dry to obtain 10.6 g of silymarin , detected by HPLC, the purity is 98.9%.

Embodiment 3

[0022] Get milk thistle fruit fine powder (60 orders of particle size) 10Kg, join in CO 2 In the supercritical extractor, methanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 4%, the extraction pressure is 30MPa, the temperature is 45°C, and CO 2 The flow rate is 2ml / g crude drug / min, the extraction time is 200min, the extract is obtained, add acetone, stir to dissolve, filter, take the filtrate, concentrate, inject high-efficiency countercurrent extractor, and use water-acetone-chloroform (1:5:2) Solvent system, the lower phase is the stationary phase, the upper phase is the mobile phase, collect the silymarin segment, concentrate, precipitate crystals, separate the crystals, add acetone-petroleum ether (1:1) for recrystallization, separate, wash, and dry to obtain 10.3 g of silymarin , detected by HPLC, the purity is 99.8%.

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Abstract

The invention relates to a method for preparing Silymarin. The method has the advantages that the operation is simple and convenient, the pollution is low and the equipment investment is small. The technological steps are that: Silybum marianum fine powder is taken and is added in a CO2 supercritical extractor, methanol is used as entrainer, the entrainer accounts for 2-6 percent of the total volume of extraction solvent, the extraction pressure is 10-40MPa, the extraction temperature is 30-60 DEG C, CO2 flow is 1-5ml per gram crude drug per minutes, the extraction time is 150-250min, the extract is obtained, acetone is added, agitation is conducted to enable the acetone to be dissolved, filtration is conducted, the filtered liquid is obtained and is concentrated, the obtain liquid is filled in a high-efficiency countercurrent extractor, water-acetone-chloroform (1:5:2) solvent system is used, the bottom phase is a fixed phase, the top phase is a flowing phase, Silymarin segments are collected and are concentrated, crystals are precipitated and are separated, and acetone-petroleum ether (0.5-2:1) are added for recrystallization. The invention has the advantages that the purity of the prepared Silymarin is high and the industrialization amplification can be realized easily.

Description

technical field [0001] The invention relates to a method for preparing silymarin, in particular to a method for extracting silymarin from plants. Background technique [0002] Silymarin, synonym: Silymarin, silymarin, etc. Molecular formula: C 25 h 22 o 10 , molecular weight: 482.443, CAS accession number: 22888-70-6, the structural formula is as follows: [0003] [0004] Silymarin is a natural compound with hepatoprotective and other physiological activities, mainly found in Silybum marianum (L.), a plant of the genus Silybum in the family Asteraceae. [0005] In the prior art, the extraction and separation methods of silymarin mainly use organic solvent methods, etc., but the content of silymarin obtained by these extraction processes is low, the pollution in the production process is serious, and it is not conducive to large-scale production operations. Contents of the invention [0006] The technical problem to be solved by the present invention is to provide ...

Claims

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Application Information

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IPC IPC(8): C07D407/04
CPCY02P20/54
Inventor 王琳范淦彬
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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