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Preparation method of silymarin

A technology for silymarin and silymarin, which is applied in the field of preparation of extracting high-purity silymarin, can solve the problems of affecting the color and yield of silymarin products, complicated impurity removal processes, solvent residues and the like, and achieves simplified preparation method, improved extraction rate, enhanced The effect of solubility

Active Publication Date: 2016-04-20
内蒙古昶辉生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Foreign patents use oil extraction method or petroleum ether and n-hexane to remove oil from milk thistle, which not only affects the color and yield of silymarin products, but also easily produces solvent residues. It takes a lot of effort to make the final product meet the standard of less than 100 ppm solvent residue complex impurity removal process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The seed coats of 10 tons of milk thistle seeds are removed by shelling machines, and the seed coats are collected to obtain 4.5 tons of seed coats. After 15 minutes of ultraviolet irradiation, the seed coats are put into the enzymatic reaction tank, softened by steam at 100°C for 20 minutes, and the water content of the material is discharged. About 8%, lower the temperature to 25°C, add 1.5% raw material weight of cellulase: pectinase: alkaline protease (5:4:1) compound enzyme, run the agitator, and enzymatically hydrolyze for 40 minutes. Move the enzymatically hydrolyzed raw materials into the material grid of the horizontal extractor, the charging amount is 70-80% of the material grid, the extraction temperature is 25°C, the rotation speed is 1r / 60-120min, spray continuously with absolute ethanol Drenched, extracted for 3 hours to obtain the extract; the extract was concentrated to 10m 3 Afterwards, the solvent was evaporated by vacuum drying, washed with 8 times th...

Embodiment 2

[0030] The seed coats of 25 tons of milk thistle seeds are removed by shelling machine, and the seed coats are collected to obtain 9.5 tons of seed coats. After 20 minutes of ultraviolet irradiation, the seed coats are put into the enzymatic reaction tank, softened by steam at 110°C for 15 minutes, and the water content of the material is discharged. About 9%, lower the temperature to 30°C, add 2.0% raw material weight of cellulase: pectinase: alkaline protease (5:4:1) compound enzyme, run the agitator, and enzymolyze for 30 minutes. Move the enzymatically hydrolyzed raw material into the material grid of the horizontal extractor, the loading amount is 70-80% of the material grid, the extraction temperature is 30°C, the rotation speed is 1r / 60-120min, spray continuously with absolute ethanol Drenched and extracted for 5 hours to obtain the extract; the extract was concentrated to 10m 3 Afterwards, the solvent was evaporated by vacuum drying, and washed with 6 times of water to...

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Abstract

The invention relates to a preparation method for extracting high-purity silymarin from silybum marianum seed husk. The preparation method comprises the following steps: separating silybum marianum seeds from seed husk, radiating by ultraviolet, carrying out the enzymolysis, extracting by absolute ethyl alcohol, volatilizing a solvent in an extracting solution, and washing solids to obtain a silymarin crude product; dissolving in absolute ethyl alcohol, obtaining supernatant, treating by adopting the reversed phase partition chromatography, carrying out the gradient elution by using water-ethyl alcohol, collecting eluate of the absolute ethyl alcohol part, concentrating the eluate, and vacuum-drying by virtue of microwaves to obtain a product. The method is simple in process, high in production efficiency and simple to operate, the product purity can reach up to 93 percent or more, and basically no solvent remains.

Description

technical field [0001] The invention relates to a preparation method of silymarin, in particular to a preparation method of extracting high-purity silymarin from milk thistle seeds. Background technique [0002] Silymarin (silmyarin) is a mixture of flavonoid lignans formed by the condensation of dihydroflavonols and phenylpropanoid derivatives. Also known as milk thistle seeds), the main components are silybin (silibinin, silibinin), isosilybin (isosilibinin), silychristin (siliehristin), silibinin (silidinain) four kinds of the same Separate isomers, in the form of yellow powder or crystalline powder. [0003] Studies have found that silymarin mainly has the function of protecting the liver and gallbladder, and can protect liver cells from toxic substances, especially alcohol and environmental pollutants (pesticides, heavy metals, etc.) that invade and damage the liver. It is clinically used to treat hepatitis, cholecystitis, etc.; It also has strong anti-oxidation, free...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D407/04
CPCC07D407/04
Inventor 马亚琼赵永强徐旭贾洪涛张成亮
Owner 内蒙古昶辉生物科技股份有限公司
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