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Method for extracting astilbin from china root

A technology of astilbin and smilax, which is applied in the field of extracting astilbin, which can solve the problems of increased environmental burden, low specificity, and high production cost, and achieves the effects of easy industrial scale-up, high purification specificity, and low cost

Inactive Publication Date: 2012-05-02
苏州北商智业管理咨询有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] There are few reports about extracting astilbin in plants, and most processes are extracted as a part of total glycosides, and the specificity is not strong. The method of extracting and extracting only obtains flavonoid saponin mixture, and the Chinese patent of publication number CN101732540A "method for determining the active components of total glycosides in ethanol aqueous extract of Smilax smilax" obtains glycosides through alcohol extraction and silica gel chromatography, but falls The content of aspartame is relatively low; some of them have only studied part of the purification method, and cannot constitute a complete process, such as Wang Jinhuang et al. , such as Chen Xing et al. "HPLC Determination of Astilbin in Smilax Smilax", Zhang Xiaoyan, etc. "High Performance Liquid Chromatography Determination of Astilbin in Smilax Smilax Medicinal Materials"
[0012] Publication No. CN1724552 "A Preparation Method for Astilbin" describes the separation method of astilbin by macroporous adsorption resin and polyamide, which has reference significance for the design of this process. However, there are many impurities carried after extraction by percolation, which makes The amount of organic solvent in the subsequent steps increases, which brings about the increase of production cost and the aggravation of environmental burden

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  • Method for extracting astilbin from china root

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Take 2 kg of Smilax cocos (astilbin content 0.23%), grind it into 20 meshes, add 16 L of water, reflux extraction for 1 hour, extract 3 times, and combine the extracts. The extract was concentrated in vacuum to 1 / 4 of the original volume, 2% sodium chloride was added while it was hot, acidified with hydrochloric acid with stirring until the pH was 2, the flavonoids were precipitated, and filtered. The filtrate was further diluted with water and filtered. Combine the two filter cakes and add 2 times the amount of ethyl acetate to degrease. The dry degreased solid is saturated and dissolved with 90% ethanol. The sample is mixed with AB-8 macroporous resin, and the water-soluble impurities are first eluted with water at a flow rate of 2BV / h until it flows The product was colorless, and then eluted with 10% ethanol at a flow rate of 2BV / h until astilbin was detected, and finally eluted with 60% ethanol at a flow rate of 2BV / h to obtain astilbin eluate. Astilbin was deliqui...

Embodiment 2

[0036] Take 2 kg of Smilax cocos (astilbin content 0.28%), grind it into 20 meshes, add 12 L of water, reflux extraction for 2 hours, extract twice, and combine the extracts. The extract was concentrated in vacuum to 1 / 5 of the original volume, 3% sodium chloride was added while it was hot, acidified with hydrochloric acid to pH 2 after stirring, and the flavonoids were precipitated, and filtered. The filtrate was further diluted with water and filtered. Combine two filter cakes and add 3 times the amount of ethyl acetate to degrease, and the dried degreased solid is saturated and dissolved with 95% ethanol, and the mixed sample is saturated with AB-8 macroporous resin for adsorption, and the water-soluble impurities are firstly eluted with water at a flow rate of 2BV / h Until the effluent is colorless, then elute with 30% ethanol at a flow rate of 2BV / h until astilbin is detected, and finally use 80% ethanol at a flow rate of 2BV / h to wash off astilbin to obtain an astilbin el...

Embodiment 3

[0038] Take 2 kg of Smilax cocos (astilbin content 0.3%), pulverize into 30 mesh, add 15 L of water, reflux extraction for 1 hour, extract 3 times, and combine the extracts. The extract was concentrated in vacuum to 1 / 4 of the original volume, 2% sodium chloride was added while it was hot, acidified with hydrochloric acid to pH 1 after stirring, the flavonoids were precipitated, and filtered. The filtrate was further diluted with water and filtered. Combine the two filter cakes and add 2 times the amount of ethyl acetate to degrease. The dry degreased solid is saturated and dissolved with 90% ethanol, and the mixed sample is saturated with HPD-400 macroporous resin for adsorption. First, water-soluble impurities are eluted with water at a flow rate of 2BV / h Until the effluent is colorless, elute with 50% ethanol at a flow rate of 2BV / h until astilbin is detected, and finally use 90% ethanol at a flow rate of 2BV / h to wash off astilbin to obtain an astilbin eluate. Astilbin wa...

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Abstract

The invention relates to a method for extracting an astilbin from a china root. The method comprises the following steps: taking the china root as a raw material; extracting in a manner of water backflow; adding salt and acid, and depositing flavonoid glycoside; after degreasing deposition, dissolving in alcohol and adding a macro-porous resin column; utilizing water to remove impurities; utilizing the alcohol to elute in a gradient form; collecting the astilbin stream; and concentrating and re-crystallizing, thereby obtaining a product. The method for producing the astilbin has the advantages of convenience in operation, low cost, environmental friendliness, strong technical specificity, high yield and high purity.

Description

Technical field: [0001] The invention relates to a method for extracting astilbin from Smilax smilax, especially a method for purifying astilbin by water extraction, acid precipitation, macroporous resin separation and recrystallization. Background technique: [0002] Smilax glabra Roxb is the dried rhizome of Smilax glabra Roxb, a plant of the genus Smilax in the family Liliaceae. It has the functions of dehumidification, detoxification, and joint benefit. The main active ingredients of Smilax smilax and its extracts are saponins and flavonoids. It is reported that the water extract of Smilax smilax has obvious anti-inflammatory effect, and astilbin extracted and separated from Smilax smilax has obvious diuretic and analgesic effects. [0003] Astilbin (astilbin) is a compound extracted from the plant Astilbin for the first time by Kozo Hayashi and Kazuhiko Ouchi in 1950. According to literature reports, astilbin has a variety of significant biological activities, includin...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
Inventor 李法庆钱钰
Owner 苏州北商智业管理咨询有限公司
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