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Preparation method of high-purity silibinin

A silybin and high-purity technology, which is applied in the field of preparation of high-purity silibinin, can solve the problems that the product is affected by the quality of the crude product, and achieve the effect of method system coordination, less time and simple method

Active Publication Date: 2020-03-13
HUNAN QIANJIN XIELI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method is mainly the refining and purification process of silybin, and the resulting product is affected by the quality of the crude product

Method used

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  • Preparation method of high-purity silibinin
  • Preparation method of high-purity silibinin

Examples

Experimental program
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Effect test

Embodiment 1

[0034] 1. Superfine pulverization: 30kg of milk thistle is added to a superfine pulverizer for superfine pulverization, and after pulverization, pass through a 120-mesh sieve to obtain pulverized materials.

[0035] 2. Countercurrent extraction: Put the pulverized material into a tank-type countercurrent extraction equipment, heat it to 60°C with 60L ethyl acetate for 2 hours of circulation extraction, and concentrate the extract after extraction to obtain 2.52kg of crude silymarin.

[0036] 3. Recrystallization: Dissolve 2.52kg of crude silymarin in 15L of acetone, stir while heating until completely dissolved, add 0.252kg of activated carbon for decolorization for 0.5h, and cool to obtain silymarin in acetone solution. Add the silymarin solution in acetone to 100L of water, stir well, let it stand, and filter to obtain the wet product of silymarin.

[0037] 4. Drying and pulverization: dry the wet product of silibinin in a vacuum drying oven, and then pulverize it to obtain ...

Embodiment 2

[0039] 1. Superfine pulverization: 30kg of milk thistle is added to a superfine pulverizer for superfine pulverization. After pulverization, pass through a 70-mesh sieve to obtain pulverized materials.

[0040] 2. Countercurrent extraction: put the pulverized material into the tank-type countercurrent extraction equipment, use 45L of ethyl acetate to heat to 80°C for 3 hours of circulation extraction, after extraction, concentrate the extract to obtain 2.46kg of crude silymarin.

[0041] 3. Recrystallization: Dissolve 2.46 kg of crude silymarin in 17 L of acetone, stir while heating until completely dissolved, add 0.492 kg of activated carbon for decolorization for 0.5 h, and cool to obtain a solution of silymarin in acetone. The silymarin acetone solution was added to 102L of water, fully stirred, allowed to stand, and filtered to obtain a wet product of silymarin.

[0042] 4. Drying and pulverization: dry the wet product of silibinin in a vacuum drying oven, and then pulveri...

Embodiment 3

[0044] 1. Superfine pulverization: 30kg of milk thistle is added to a superfine pulverizer for superfine pulverization, and after pulverization, pass through a 120-mesh sieve to obtain pulverized materials.

[0045] 2. Countercurrent extraction: put the pulverized material into a tank-type countercurrent extraction equipment, use 75L of ethyl acetate to heat to 50°C for cyclic extraction for 1 hour, and concentrate the extract after extraction to obtain 2.54kg of crude silymarin.

[0046] 3. Recrystallization: Dissolve 2.54 kg of crude silymarin in 13 L of acetone, stir while heating until completely dissolved, add 0.254 kg of activated carbon for decolorization for 1 hour, and cool to obtain a solution of silymarin in acetone. The silymarin acetone solution was added to 104L of water, fully stirred, allowed to stand, and filtered to obtain a wet product of silymarin.

[0047] 4. Drying and pulverization: dry the wet product of silibinin in a vacuum drying oven, and then pulve...

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Abstract

The invention discloses a preparation method of high-purity silybin. The method comprises the following steps: (1) superfinely grinding: superfinely grinding Silybum marianum to 70-120 meshes, and screening the ground Silybum marianum to obtain a ground material; (2) performing countercurrent extraction: adding the ground material into ethyl acetate, heating the obtained solution to 50-80 DEG C, carrying out circulating extracting for 1-3 h, and concentrating the obtained extract after extraction to obtain crude silymarin; (3) recrystallizing: adding the crude silymarin into acetone, dissolving the crude silymarin to obtain a silymarin dissolved acetone solution, adding the silymarin dissolved acetone solution into water, and filtering the obtained solution to obtain a wet silybin product;and (4) drying and crushing the wet silybin product. The method has the advantages of simplicity in operation, and short time, and the obtained silibinin has the advantages of high extraction rate, few solvent residues and high purity.

Description

technical field [0001] The invention belongs to the technical field of natural organic chemistry. More specifically, it relates to a preparation method of high-purity silibinin. Background technique [0002] Silybin is a flavonoid compound extracted and isolated from the fruit of the Compositae plant Silybum marianum. It has obvious effects of protecting and stabilizing liver cell membranes, improving liver function and producing enzyme-lowering effects. And not prone to enzyme rebound. Silybin is the main active ingredient of silymarin. Silymarin can stabilize liver cell membranes, maintain the integrity of liver cells, prevent toxins from penetrating and destroying the liver, and accelerate the synthesis of DNA (deoxyribonucleic acid) in liver cells, preventing liver damage. Cirrhosis, fatty liver, cholangitis, psoriasis and other diseases, and at the same time inhibit the growth and differentiation of liver cancer, prostate cancer, breast cancer and cervical cancer cell...

Claims

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Application Information

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IPC IPC(8): C07D407/04
CPCC07D407/04
Inventor 曹瑞任超彭华军周超刘如斯邹洋廖爱玲
Owner HUNAN QIANJIN XIELI PHARMA CO LTD
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