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Preparation method of kutkin I crystal

A technology of picroside and picroside, which is applied in the field of purification and preparation of picroside I monomer, can solve the problems of not obtaining pure picroside I, and no patent for picroside I, etc.

Active Publication Date: 2015-03-11
济南东源生物医药技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After searching for its medical use and preparation process, patents have been applied for (Chinese patent application number: 200410098646.4[1]; 200710164321.5[2]; 201310618996.8[ 3], U.S. Patent No.: US005145955[4]) The methods used for preparation are chromatography, macroporous adsorption, lead salt precipitation and other methods, and the obtained substance is amorphous or combined with other substances None of the mixed crystals obtained the crystallization products of berberine Ⅰ, and no patents on the crystallization of berberine Ⅰ were found after searching, and no relevant academic papers were published.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1. Get 10 g of Coptis chinensis extract with a purity of 80% through two column chromatography, dissolve in 100 ml of ethanol with a concentration of 85% at 50 ° C, filter while hot, and place the filtrate in In the refrigerator at -13°C, after 24 hours, the crystals of berberine I were filtered out, and freeze-dried to obtain 4.5 g of berberine I with a purity of 93%.

Embodiment 2

[0021] Example 2. Get 10 g of Coptis chinensis extract with a purity of 85% through two column chromatography, dissolve in 130 ml of ethanol with a concentration of 95% at 20 ° C, filter while hot, and place the filtrate in In a constant-temperature refrigerator at 0°C, after 24 hours, filter out the crystals of berberine I, and dry under reduced pressure at 60°C to obtain 6.33 g of berberine I with a purity of 96%.

Embodiment 3

[0022] Example 3. Take 10 g of Coptis chinensis extract with a purity of 75% through two column chromatography, dissolve it in 50 ml of absolute ethanol at 30°C, filter it while it is hot, and place the filtrate at a constant temperature of 4°C In the refrigerator, after 24 hours, the crystals of berberine I were filtered out, and freeze-dried to obtain 3 g of berberine I with a purity of 93%.

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PUM

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Abstract

The invention relates to a purification method of kutkin I, which comprises the following step: by using a rhizoma picrorhizae extract with the kutkin I purity of not lower than 75% as a raw material and ethanol or an ethanol-water mixture as a solvent, carrying out crystallization and recrystallization purification on the kutkin I. The method is simple and convenient, has the characteristics of favorable reproducibility, high purity, high yield and high operability, and is especially suitable for large-scale industrialization.

Description

technical field [0001] The invention relates to a method for purifying and preparing a pubetroside I monomer. technical background [0002] Huhuanglian is a traditional Chinese medicine in my country, which was first recorded in "Tang Materia Medica". Hemorrhoids swelling and pain etc. The main chemical components are iridoid glycosides, cucurbitacins, phenylethanol glycosides and phenolic glycosides. Picroside I (Picroside I) is one of the main active ingredients of iridoid glycosides. According to reports, berberine Ⅰ has pharmacological effects such as protecting the liver and gallbladder, and protecting the nerves. After searching for its medical use and preparation process, a patent has been applied for (Chinese patent application number: 200410098646.4 [1] ;200710164321.5 [2] ; 201310618996. 8 [3] , U.S. Patent No.: US005145955 [4] ) is prepared by methods such as chromatography, macroporous adsorption, lead salt precipitation, etc., and the obtained substance is...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
CPCC07H1/08C07H17/04
Inventor 刘培冉杨涛贺灵剑刘文卉孙士青
Owner 济南东源生物医药技术有限公司
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