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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 difficult degreasing and separation and purification in the traditional silybin preparation method, and improves the obtained water content. Silybin content

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Example 1: Feed 600g of milk thistle shell powder crushed through 16 meshes, add 1020g of ethyl acetate to dissolve it, reflux to extract the total flavonoids for 2 hours, then add 780g of ethyl acetate, and reflux to extract the total flavonoids for 16 hours , combined the total flavonoids extracted twice, and collected ketones in a vacuum to obtain 82 g of total flavonoids.

[0024] 82g of total flavones were dissolved by adding purified water 5 times the mass of total flavones, stirred in a water bath and allowed to stand for 1 hour, and 246g of ethanol solution with a concentration of 50% was added to the precipitate to dissolve it to obtain 70g of silybin crude product I; Add 210g of 65% ethanol solution to the crude silibinin I to dissolve, and crystallize for 24 hours to obtain 52g of the crude silibinin II; add 520g of absolute ethanol to the crude silibinin II to dissolve, and then Microporous filtration while hot, concentrate the filtrate to about 20% of the t...

Embodiment 2

[0025] Embodiment 2: Get 600g milk thistle shell feed intake, add 1020g ethyl acetate and dissolve it, reflux extracts total flavonoids for 2 hours, then add 780g ethyl acetate, reflux extracts total flavonoids for 16 hours, merge the total flavonoids extracted twice Liquid, ketones were collected in vacuum to obtain 78g total flavonoids.

[0026] 78g total flavones were dissolved by adding purified water 5 times the total flavonoids mass, stirred in a water bath and allowed to stand for 1 hour, and the precipitate was dissolved by adding 234g of 50% ethanol solution to obtain 65g of silybin crude product I; Add 210g of ethanol solution with a concentration of 65% to the crude silibinin I to dissolve, crystallize for 24 hours to obtain 48g of the crude silibinin II; add 480g of absolute ethanol to the crude silibinin II to dissolve, and after the Microporous filtration while hot, concentrate the filtrate to about 20% of the total volume of crude silibinin II and the added abso...

Embodiment 3

[0027] Example 3: Feed 300 g of milk thistle shell powder crushed through 16 meshes, add 510 g of ethyl acetate to dissolve it, reflux to extract the total flavonoids for 2 hours, then add 390 g of ethyl acetate, and reflux to extract the total flavonoids for 16 hours , combined the total flavonoids extracted twice, and collected the ketones in a vacuum to obtain 45 g of total flavonoids.

[0028] Add purified water 3 times the mass of total flavonoids to dissolve 45g of total flavonoids, stir in a water bath and let stand for 1 hour, take the precipitate and add 135g of ethanol solution with a concentration of 50% to dissolve it, and obtain 34g of silybin crude product I; Add 102g of 65% ethanol solution to the crude silibinin I to dissolve, crystallize for 24 hours to obtain 25g of the crude silibinin II; Microporous filtration while hot, concentrate the filtrate to about 20% of the total volume of crude silibinin II and the added absolute ethanol, place at room temperature ...

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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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