New method for extracting silymarin from silybum mariamum

A milk thistle and water extraction technology, which is applied in the field of synergistic extraction of silymarin by using enzyme-continuous countercurrent ultrasound, can solve the problems of unfavorable industrial production, long production cycle, and difficult production, and achieve low production cost, increase extraction rate, and increase The effect of solubility

Inactive Publication Date: 2014-12-24
NANJING BIAOKE BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the traditional methods of extracting silymarin in China mostly use methods such as organic solvent percolation and heat reflux, but these methods generally have problems such as high energy consumption, long production cycle, and low yield.
In addition, there are patent reports using supercritical carbon dioxide extraction to extract silymarin, but high temperature and high pressure production is difficult and dangerous, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The dried silymarin seeds were pressed to remove oil, dried at 60°C, pulverized, and 5 times of 80% ethanol was added to 1kg of pulverized silymarin seeds, and then 0.5% of the raw material weight of compound enzyme (cellulase) was added. : hemicellulase: pectinase (0.5:0.3:0.2), stir evenly, continuously countercurrent ultrasonic extraction at 60°C, 60KHz for 2h, filter, add the filtrate to the pretreated A8-8 macroporous adsorption resin column for adsorption, first The resin column was washed with water, then 5BV of 60% ethanol was added to elute the active ingredients, the eluate was collected, concentrated under reduced pressure, and dried to obtain 18.1 g of silymarin. After UV detection, the total flavonoid content was 80.3%.

Embodiment 2

[0019] The dried milk thistle seeds were pressed to remove oil, dried at 60°C, and pulverized. 8 times of 70% ethanol was added to 1kg of pulverized milk thistle seeds, and then 1.0% of the raw material weight of compound enzyme (cellulase) was added. : hemicellulase: pectinase (0.5:0.3:0.2), stir evenly, continuously countercurrent ultrasonic extraction at 55°C, 80KHz for 2.5h, filter, add the filtrate to the pretreated NKA-9 macroporous adsorption resin column for adsorption, First wash the resin column with water, then add 70% ethanol of 8BV to elute the active ingredients, collect the eluate, concentrate under reduced pressure, and dry to obtain 20.4g of silymarin. After UV detection, the total flavonoid content is 84.7%.

Embodiment 3

[0021] The dried milk thistle seeds were pressed to remove oil, dried at 60°C, pulverized, and 10 times of 60% ethanol was added to 1 kg of pulverized milk thistle seeds, and then 1.5% of the raw material weight of compound enzyme (cellulase) was added. : hemicellulase: pectinase (0.5:0.3:0.2), stir evenly, continuously countercurrent ultrasonic extraction at 50°C, 70KHz for 3h, filter, add the filtrate to the pretreated D-101 macroporous adsorption resin column for adsorption, first The resin column was washed with water, then 10BV of 80% ethanol was added to elute the active ingredients, the eluate was collected, concentrated under reduced pressure, and dried to obtain 19.8 g of silymarin. The total flavonoid content was 81.9% by UV detection.

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PUM

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Abstract

The invention discloses a new method for extracting silymarin from silybum mariamum, and particularly relates to a method for synergistically extracting the silymarin through enzyme-continuous counterflow ultrasonics. The method comprises the following steps of squeezing a dried silybum mariamum seed as a raw material to remove oil; drying at 60 DEG C; crushing; soaking by adopting ethanol, and adding a complex enzyme for enzymolysis; carrying out continuous counterflow ultrasonic extraction; filtering; purifying pretreated macroporous adsorption resin positioned above filter liquor; eluting by adopting a solvent; and concentrating to obtain the silymarin. The method disclosed by the invention enhances the dissolution rate of an effective component through the synergistic effect of biological enzyme wall-breaking and the continuous counterflow ultrasonic and has the advantages of no toxicity, moderate reaction condition, high extraction rate, short extraction time and low extraction cost, and is suitable for industrialized production.

Description

technical field [0001] The invention belongs to the field of separation of natural products, and relates to a new method for extracting silymarin from milk thistle, in particular to a method for synergistically extracting silymarin by using enzyme-continuous countercurrent ultrasound. Background technique [0002] Silymarin is a flavonoid lignin compound extracted from the water of milk thistle fruit. The appearance is light yellow powder, insoluble in water and chloroform, soluble in methanol, ethanol, ethyl acetate, acetone and other solvents, mainly distributed in the seed shell, The content in the seed kernel is very small, mainly including compounds such as silybin, isosilibin, silybin, silybinin, etc. It has pharmacological activities of anti-hepatotoxicity, protection of liver cell membrane, and improvement of liver function. It is clinically used to treat hepatitis, cholecystitis, etc. In recent years, silymarin has been extended to the field of anti-aging and beaut...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D407/04
CPCC07D407/04
Inventor 张金芳杨存
Owner NANJING BIAOKE BIO TECH
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