Unlock instant, AI-driven research and patent intelligence for your innovation.

Industrial method for producing high-quality silymarin

A silymarin, high-quality technology, applied in the production of fat/fat, fat production, organic chemistry, etc., can solve the problems of difficult to guarantee product purity and yield, low production efficiency, and small yield

Active Publication Date: 2019-07-19
CHENGUANG BIOTECH GRP CO LTD
View PDF9 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In terms of purification, in the patent with the publication number CN107098892A, after the extract is concentrated, methanol is added to dissolve and recrystallize for 48-72 hours. The amount of methanol is large, the crystallization time is too long, and the efficiency is low
In the patent with the publication number CN107805245A, silica gel column chromatography and chloroform-methanol gradient elution can be used to prepare products with a purity of more than 99%, but the production efficiency is low and the output is small, so it is not suitable for industrial production
[0005] In a word, in the preparation method of high-purity silymarin, whether it is extracting milk thistle seeds after squeezing or using organic solvents to remove oil, the process is lengthy, time-consuming, complex and inevitably leads to large losses, and it is difficult to guarantee the purity and yield of the product
The refining process continues to use methods such as crystallization, recrystallization, and chromatographic separation, and it is difficult to guarantee the smooth realization of industrialization in terms of cost and efficiency.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Industrial method for producing high-quality silymarin
  • Industrial method for producing high-quality silymarin
  • Industrial method for producing high-quality silymarin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Take 350kg of milk thistle shell raw material, the content of silymarin in the raw material is 6.1%, after being pressed by a tablet press with a roller spacing of 0.04mm, it is continuously extracted in countercurrent with 95% acetone solution, the extraction temperature is 45°C, and the extraction process is stopped for 4 times, each stop 1.5h. Heat the extract to 60°C and concentrate to 1 / 7 of the original volume, adjust the acetone concentration in the feed solution to 38%, stand to separate the milk thistle oil, add 3 times the mass of 90% methanol to the concentrated solution after deoiling , separated after washing at 35°C, and vacuum-drying the product at 65°C to obtain 9.89kg of milk thistle product, with a silymarin content of 92.18%, and a silybin content of 88.26% in the product.

Embodiment 2

[0030] Take 500kg of milk thistle shell raw material, the content of silymarin in the raw material is 5.8%, after being compressed by a tablet press with a roller spacing of 0.04mm, it is continuously extracted in countercurrent with 96% acetone solution, the extraction temperature is 45°C, and the extraction process is stopped for 4 times, each stop 1.5h. Heat the extract to 65°C and concentrate to 1 / 8 of the original volume, adjust the acetone concentration in the feed solution to 40%, stand to separate the milk thistle oil, add 4 times the mass of 85% methanol to the concentrated solution after deoiling , separated after washing at 30°C, and vacuum-drying the product at 70°C to obtain 14.93kg of milk thistle product, with a silymarin content of 89.93%, and a silybin content of 85.47% in the product.

Embodiment 3

[0032] Take 1250kg of milk thistle shell raw material, the raw material silymarin content is 6.0%, after being compressed by a tablet press with a roller spacing of 0.04mm, it is continuously extracted in countercurrent with 98% acetone solution, the extraction temperature is 40°C, and the extraction process is stopped for 4 times, each stop 2h. Heat the extract to 60°C and concentrate it to 1 / 6 of the original volume, adjust the acetone concentration in the feed solution to 42%, stand to separate the milk thistle oil, add 95% methanol of 3 times the mass to the concentrated solution after deoiling , separated after washing at 32°C, and vacuum-drying the product at 68°C to obtain 32.68kg of milk thistle product, with a silymarin content of 88.62%, and a silybin content of 85.38% in the product.

[0033] The extraction method and extraction result of table 1 embodiment 1-3

[0034]

[0035]

[0036] It can be seen from Table 1 that by using the method of the present appl...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
thicknessaaaaaaaaaa
Login to View More

Abstract

The invention relates to an industrial method for producing high-quality silymarin. The industrial method is characterized by comprising the following steps: (a), extracting by using acetone, namely synchronously extracting silybum marianum oil and silymarin from silybum marianum shells by using the acetone to obtain an acetone extraction solution; (b), separating the silybum marianum oil from thesilymarin, namely concentrating the acetone extraction solution in the step (a) till the concentration of the acetone is 35-45% to obtain the precipitated silybum marianum oil and a silymarin-containing acetone concentrate; (c), purifying by using methanol, namely adding the methanol into the acetone concentrate for washing out impurities. By the industrial method, automatic separation of the silybum marianum oil and the silymarin can be achieved, a complicated technology of separating the silybum marianum oil from the silymarin in the prior art is omitted, a production technology is simplified and the production cost is reduced. An obtained final product has the final moisture content being lower than 5%, the silymarin product content being 85-95% and the silybin content being higher than 85%.

Description

[0001] Technical field [0002] The invention relates to an industrial method for preparing natural extracts, in particular to an industrial method for producing high-quality silymarin. Background technique [0003] Silymarin is a mixture extracted from milk thistle seeds, and silybin is its main active ingredient, which has the effect of protecting the liver. [0004] Silymarin mainly exists in the shell of milk thistle seeds. After the shells and kernels of milk thistle seeds are separated, extracting silymarin from milk thistle shells can effectively reduce the difficulty of separating silymarin, thereby simplifying the process. The milk thistle shell needs to be pretreated to improve the extraction yield. The tableting process can destroy the cell structure to a certain extent, which is more conducive to the contact between the extraction solvent and the cell content. In the patent publication No. CN105503843A, the water fly Thistle seed coats are hydrolyzed with compound...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07D407/04C11B1/10C11B3/00
CPCC07D407/04C11B1/10C11B3/00
Inventor 任世宇牛志平田洪吴迪高伟
Owner CHENGUANG BIOTECH GRP CO LTD