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A kind of preparation method of high-purity silymarin

A silymarin and high-purity technology, applied in the field of traditional Chinese medicine preparation, can solve the problems of low production capacity of silymarin, low product content, excessive organic solvent residual solvent, etc., so as to solve the problem of low product content, improve yield, high economic benefits and The effect of social benefit

Active Publication Date: 2019-05-17
ZHONGXING PHARM CO LTD JIANGSU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Purpose of the invention: In order to solve the problems of low production capacity of silymarin in the prior art, excess organic solvent residual solvent and low product content, the present invention proposes a method for preparing high-purity silymarin without degreasing steps

Method used

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  • A kind of preparation method of high-purity silymarin
  • A kind of preparation method of high-purity silymarin

Examples

Experimental program
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Effect test

Embodiment 1

[0036] Take 360g of silybum shell coarse powder after 16 mesh crushing, add 612g of mixed solvent (ethyl acetate and absolute ethanol at 2:1) to dissolve it, reflux to extract the total flavonoids for 2 hours, then add 540g of mixed Solvent (ethyl acetate and absolute ethanol at 2:1), reflux to extract the total flavonoids for 8 to 10 hours, combine the total flavonoids extracted twice, concentrate under reduced pressure in vacuo to collect ketones, and obtain 54.8 g of total flavonoids.

[0037] Add purified water that is 5 times the mass of total flavonoids, heat 54.8g of total flavonoids above 65°C to dissolve, stir for 30 minutes in a water bath and let it stand for 1 hour, leaving a precipitate that is 48g of crude silymarin I; add 144g of crude silymarin I Heat the ethanol solution with a concentration of 30% to 40-50°C, stir and dissolve, let it stand for 30 minutes, release the upper liquid, and leave the precipitate to get 37.2g of crude silymarin II; add three times t...

Embodiment 2

[0039] Get 360g of milk thistle shell feeding, add mixed solution (ethyl acetate and dehydrated alcohol by 2:1) 612g to dissolve it, reflux to extract the total flavonoids for 2 hours, then add mixed solution (ethyl acetate and anhydrous Ethanol (2:1) 540g, reflux extraction of total flavonoids for 8 to 10 hours, combined the total flavonoid liquids extracted twice, concentrated under reduced pressure in vacuo to collect ketones, and obtained 50.1g of total flavonoids.

[0040] Add purified water that is 5 times the mass of total flavonoids, heat 83.4g of total flavonoids above 65°C to dissolve, stir for 30 minutes in a water bath and let stand in a water bath for 1 hour, leaving a precipitate that is 45g of silymarin crude product I; add 135g of silymarin crude product I Heat the ethanol solution with a concentration of 30% to 40-50°C, stir and dissolve, let it stand for 30 minutes, release the upper liquid, and leave the precipitate to get 34.8g of crude silymarin II; add thr...

Embodiment 3

[0041] Embodiment 3 (comparative example, the traditional production method of silymarin): take 522g of squeezed silymarin cake, add 887.4g of ethyl acetate to dissolve it, reflux to extract the total flavonoids for 2 hours, then add 783g of ethyl acetate, reflux Extract the total flavones for 8-10 hours, combine the total flavones extracted twice, concentrate under reduced pressure in vacuo to collect ketones, and obtain 49.5 g of total flavones.

[0042]Add 49.5g of 80% ethanol to the total flavonoids, heat, dissolve and reflux for 30 minutes, stir in a water bath and let it stand for 30 minutes, slowly add 49.5g 120# gasoline into the beaker of the total flavone solution, mix for 15-30 minutes, and then pour into the Stand in the funnel for 1 hour. After standing still, concentrate the lower layer of liquid until the appearance of the extract should be yellow to brown-yellow viscous paste with a density of 1.18-1.25 (35-40°C). Put it in a drying oven and dry it at 90-100°C...

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Abstract

The invention discloses a method for preparing high-purity silymarin. The method comprises the steps as follows: silybum marianum shells are taken as the raw material, total flavonoids are extracted by a mixed solvent, then 20wt%-30wt% of ethyl alcohol is used for separation and purification, and the high-purity silymarin is obtained, wherein the mixed solvent is a mixture of ethyl acetate and absolute ethyl alcohol in a volume ratio of (2-5): 1. The method improves the productivity of silymarin, the content of UV in the obtained high-purity silymarin is larger than or equal to 80%, and exceeds the state-specified standard which is larger than or equal to 68%, while the UV content in silymarin extracted with a traditional method is only about 75%, so that the problems such as excessive residual solvents, the low product content and the like of organic solvents are solved; meanwhile, pollution to the environment by the organic solvents is reduced, and relatively high economic benefits and social benefits are achieved.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicine preparation, and in particular relates to a preparation method of high-purity silymarin. Background technique [0002] Silymarin - is a general term for flavonoids extracted from the seeds of the natural product milk thistle, and is a light yellow powdery substance. It has physiological effects such as protecting the liver, lowering blood fat, anti-oxidation, preventing diabetes, protecting myocardium, anti-platelet aggregation and anti-tumor. In the early days, silymarin was mostly extracted from milk thistle seeds by pressing whole seeds and then extracted with ethyl acetate in the cake. At present, most silymarin in China uses ethyl acetate, acetone, etc. as solvents to extract silymarin from milk thistle seeds, and then use petroleum Ether or 120# gasoline, etc. are degreased for separation and purification. [0003] The defects of the current process are mainly that the productio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D407/04
CPCC07D407/04
Inventor 徐冰
Owner ZHONGXING PHARM CO LTD JIANGSU