High-purity silymarin and preparation method thereof

A silibinin and high-purity technology, applied in the field of high-purity silibinin and its preparation, can solve problems such as difficulty in degreasing, difficulty in separation and purification, improve product quality and yield, reduce environmental pollution, and the preparation method simple effect

Active Publication Date: 2011-09-07
ZHONGXING PHARM CO LTD JIANGSU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Another object of the present invention is to provide a method for preparing high-purity silibinin, which is simple, solves the difficult problems of

Method used

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  • High-purity silymarin and preparation method thereof
  • High-purity silymarin and preparation method thereof

Examples

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Example Embodiment

[0023] Example 1: take 600g of milk thistle shell coarse powder after 16 mesh grinding, add 1020g of ethyl acetate to dissolve it, reflux and extract total flavonoids for 2 hours, then add 780g of ethyl acetate, reflux and extract total flavonoids for 16 hours , merging the total flavonoid liquids extracted twice, and collecting ketones in vacuum to obtain 82g total flavonoids.

[0024] 82 g of total flavonoids were dissolved by adding 5 times the mass of total flavonoids in purified water, stirred in a water bath and allowed to cool for 1 hour, and 246 g of ethanol solution with a concentration of 50% was added to the precipitate to dissolve it to obtain 70 g of silibinin crude product I; Add 210 g of ethanol solution with a concentration of 65% to the crude silibinin product I to dissolve, and crystallize for 24 hours to obtain 52 g of crude silibinin II; add 520 g of anhydrous ethanol to the crude silibinin product II to dissolve, and after it is completely dissolved, Micro...

Example Embodiment

[0025] Example 2: take 600g of milk thistle shell as feed, add 1020g of ethyl acetate to dissolve it, reflux and extract total flavonoids for 2 hours, then add 780g of ethyl acetate, reflux and extract total flavonoids for 16 hours, and combine the total flavonoids extracted twice Liquid, vacuum collected ketone to obtain 78g total flavonoids.

[0026] Dissolving 78 g of total flavonoids by adding purified water with an amount of 5 times the mass of total flavonoids, stirring in a water bath and allowing to cool for 1 hour, taking the precipitate and adding 234 g of ethanol solution with a concentration of 50% to dissolve it to obtain 65 g of silibinin crude product I; Add 210 g of ethanol solution with a concentration of 65% to the crude silibinin product I to dissolve, and crystallize for 24 hours to obtain 48 g of crude silibinin product II; add 480 g of anhydrous ethanol to the crude silibinin product II to dissolve, and after it is completely dissolved, Microporous filtra...

Example Embodiment

[0027] Example 3: take 300g of milk thistle shell coarse powder after 16 mesh grinding, add 510g of ethyl acetate to dissolve it, reflux and extract total flavonoids for 2 hours, then add 390g of ethyl acetate, reflux and extract total flavonoids for 16 hours , merging the total flavonoid liquids extracted twice, and collecting ketones in vacuum to obtain 45g total flavonoids.

[0028] Dissolving 45 g of total flavonoids by adding purified water that is 3 times the mass of total flavonoids, stirring in a water bath and allowing to cool for 1 hour, taking the precipitate and adding 135 g of ethanol solution with a concentration of 50% to dissolve it to obtain 34 g of silibinin crude product I; Add 102 g of ethanol solution with a concentration of 65% to the crude silibinin product I to dissolve, and crystallize for 24 hours to obtain 25 g of crude silibinin product II; add 250 g of absolute ethanol to the crude silibinin product II to dissolve, and after it is completely dissolv...

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Abstract

The invention discloses a high-purity silymarin and a preparation method thereof. The content of the high-purity silymarin is 97-101%. The preparation method of the high-purity silymarin comprises the following steps of: taking a silymarin shell as a raw material; adding ethyl acetate for dissolving the silymarin shell; extracting total flavones; collecting flavones in vacuum; and dissolving, extracting, filtering and drying the total flavones to obtain the high-purity silymarin. The invention has the advantages that on the basis of a silymarin seed, shell and kernel separating technology, the silymarin shell is used as the raw material for preparing the silymarin, the total flavones are extracted and then separated and purified by using ethanol with different concentration, and a recrystallization technology is adopted to prepare the high-purity silymarin. Because 99% of silymarin oil exists in the silymarin kernel, the silymarin shell is used for extracting the total flavones, the grease is little, a traditional method in which gasoline, petroleum ether and other organic solvents are used for degreasing is not required, and impurity interference, separation and purification difficulty and environment pollution are reduced. The preparation method disclosed by the invention is relatively simple, and the product quality and yield of the high-purity silymarin are greatly improved.

Description

technical field [0001] The invention relates to silibinin and a preparation method thereof, in particular to high-purity silybin and a preparation method thereof. Background technique [0002] Silybin, chemical name: 2α-[2,3-trans-2,3-dihydro-3-(4-hydroxy-3-methoxyphenyl)-2-hydroxymethyl-1,4 -Benzodioxane-6-yl]-2,3-dihydro-3β,5,7-trihydroxy-4H-1-benzopyran-4-one-hydrate, molecular formula: C 25 h 22 o 10 ·H 2 O, molecular weight: 500.47. [0003] Silybin is usually used as a raw material drug. The series of products made from silibinin have the functions of protecting the liver and repairing liver cell membranes. After years of clinical evidence, the curative effect of this type of product has been proven, and no toxicity has been found so far. side effect. With the deepening of research, more important activities of silibinin are gradually revealed. Modern research proves that high-purity silibinin not only has the function of protecting liver and liver, but also has ...

Claims

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Application Information

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IPC IPC(8): C07D407/04
Inventor 戴军武俊明徐冰
Owner ZHONGXING PHARM CO LTD JIANGSU
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