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Separation and preparation method of patuletin-3-O-glucoside and astragalin

A technology of glucoside and milkvetch glycoside, which is applied in the preparation of sugar derivatives, chemical instruments and methods, and sugar derivatives, and can solve the problems of high cost, cumbersome process, and low recovery rate

Inactive Publication Date: 2009-10-28
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] According to the existing literature, the method of column chromatography and high performance liquid chromatography is used for separation, and the crude product is separated from ethanol through a reversed-phase silica gel column, a carbon-octave column, and a Sephadex LH-20 column to obtain tagetin-3-O-glucose Glycoside and astragalin, or obtain tagetin-3-O-glucoside and astragalin after repeated silica gel column separation, the process is cumbersome, the cost is high, and the recovery rate is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Select n-hexane-ethanol-water on a semi-preparative countercurrent chromatograph to separate and purify the Flavonium chrysanthemum extract (the raw material of Ethanol chrysanthemum extracted by ethanol), first configure the above solvent components in a separatory funnel according to the volume ratio of 10:1:10, shake Let it stand for layering. After equilibrating for a period of time, separate the upper phase and the lower phase, take the lower phase as the stationary phase, and the upper phase as the mobile phase. A semi-preparative high-speed countercurrent chromatograph is used, equipped with NS-1007 pump, 20mL injection valve, polytetrafluoroethylene column with a column volume of 240mL, 8823A-UV ultraviolet detector, and Yokogawa 3057 portable recorder. Weigh 400 mg of ethanol-extracted chrysanthemum raw material and dissolve it in 20 mL of mobile phase for use. Before sample injection, fill the entire column with the stationary phase, adjust the speed of the m...

Embodiment 2

[0017] Butyl acetate-methanol-water was used to separate the extract of Flavonium chrysanthemum on a semi-preparative countercurrent chromatograph. Firstly, the above-mentioned solvent components were arranged in a separatory funnel according to a volume ratio of 30:1:30, shaken up, and then stood to separate layers. After equilibrating for a period of time, separate the upper phase and the lower phase, take the lower phase as the stationary phase, and the upper phase as the mobile phase. A semi-preparative high-speed countercurrent chromatograph is used, equipped with NS-1007 pump, 20mL injection valve, polytetrafluoroethylene column with a column volume of 240mL, 8823A-UV ultraviolet detector, and Yokogawa 3057 portable recorder. Weigh 100mg of the crude product of chrysanthemum extracted by ethanol and dissolve it in 20mL of mobile phase for use. Before sample injection, fill the entire column with stationary phase, adjust the host speed to 1000rpm, and pump the mobile phas...

Embodiment 3

[0019] Take the ethyl acetate-methanol-water fraction on an analytical counter-current chromatograph to separate the Flavonium extract. Firstly, the above-mentioned solvent components were arranged in a separatory funnel according to a volume ratio of 10:1:30, shaken up and left to stand to separate layers. After equilibrating for a period of time, separate the upper phase and the lower phase, take the lower phase as the stationary phase, and the upper phase as the mobile phase. A semi-preparative high-speed countercurrent chromatograph is used, equipped with NS-1007 pump, 20mL injection valve, polytetrafluoroethylene column with a column volume of 240mL, 8823A-UV ultraviolet detector, and Yokogawa 3057 portable recorder. Weigh 400mg of the crude product of Ethanol-extracted Chrysanthemum chrysanthemum and dissolve it in 10mL of mobile phase for later use. Before sample injection, fill the entire column with the stationary phase, adjust the speed of the main engine to 800rpm,...

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PUM

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Abstract

The invention relates to a separation and preparation method of patuletin-3-O-glucoside and astragalin. The method adopts counter current chromatography to separate and prepare the patuletin-3-O-glucoside and astragalin from alcohol reflux extracts of plant flaveria bidentis; a solvent thereof comprises three components, namely ether or n-alkane or fatty ester, acetonitrile or fatty alcohol or aliphatic ketone and water; the volume ratio is as follows in sequence: 30 to 10:1:30 to 10; and the method is applicable to prepare the monomeric patuletin-3-O-glucoside and astragalin by various types of counter current chromatographs, and can be directly filled with large amount of crude products or synthetic mixtures with the separation purity of more than 95 percent.

Description

technical field [0001] The invention relates to a method for separating and preparing high-purity monomer tagetine-3-O-glucoside and milkvetch glycoside from the extract of alien invasive plant chrysanthemum chrysanthemum by using high-speed countercurrent chromatography. Background technique [0002] Flaveria bidentis (L.) Kuntze is an annual herb of the genus Flaveria in the Asteraceae family, which originated in South America. Chrysanthemum chrysanthemum plants are tall and dense, with amazing seed yield, strong reproductive ability and adaptability. It can invade various habitats such as farmland, roadside, and wasteland, and can inhibit the growth of other plants through allelopathy, thereby quickly occupying ecological niches. In addition to its origin, Chrysanthemum chrysanthemum is invasive in other countries and regions, posing a great threat to the ecological environment and agricultural production, and is a highly dangerous alien invasive plant. Since it was firs...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08B01D15/08
Inventor 魏芸谢倩倩
Owner BEIJING UNIV OF CHEM TECH
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