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Method for separating and purifying stilbene glucoside monomers

A technology for stilbene glycosides and crude stilbene glycosides, which is applied in the field of separation and purification of stilbene glycoside monomers by high-speed countercurrent chromatography, can solve the problems of large solvent consumption, expensive instruments, cumbersome operation steps, etc., and achieves the goal of preparing The effect of large quantity, good recovery rate and advanced technology

Inactive Publication Date: 2012-08-01
BEIJING CENT FOR PHYSICAL & CHEM ANALYSIS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The existing preparation and separation methods of stilbene glycoside monomer components mostly adopt simple solvent extraction and column chromatography separation and purification methods, which are widely used and have the advantages of large sample processing capacity, but the disadvantage of the above methods is that the operation The steps are cumbersome, the sample recovery rate is low, and the purity of the obtained samples is not high, etc.
In addition, there is a high-purity liquid chromatographic separation method to obtain stilbene glycoside monomer components with high purity, but this method is expensive in terms of instrument cost and large solvent consumption, which restricts the development of this technology

Method used

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  • Method for separating and purifying stilbene glucoside monomers
  • Method for separating and purifying stilbene glucoside monomers
  • Method for separating and purifying stilbene glucoside monomers

Examples

Experimental program
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Effect test

Embodiment 1

[0026] (1) Mix ethyl acetate, ethanol and water in a volume ratio of 15:1:15, place in a separatory funnel, shake fully and leave to separate layers, take the upper layer solution as the stationary phase and the lower layer solution as the mobile phase, Standby; dissolve 300mg of crude stilbene glycosides in 20mL of the lower layer solution, and set aside;

[0027] (2) Use semi-preparative high-speed countercurrent chromatograph, with the ternary solvent system that above-mentioned ethyl acetate, ethanol and water are formed as separation solvent system; In the chromatographic column of high-speed countercurrent chromatograph, be full of stationary phase, then adjust rotating speed 800r / Min to make the host rotate, set the temperature of the constant temperature water bath to 20°C, set the detection wavelength of the ultraviolet detector to 280nm, and then pump the mobile phase into the chromatographic column at 2.5mL / min; Crude product of stilbene glycosides (sample injectio...

Embodiment 2

[0033] (1) Mix ethyl acetate, ethanol and water at a volume ratio of 35:1:35, place in a separatory funnel, shake fully and leave to separate layers, take the upper layer solution as the stationary phase and the lower layer solution as the mobile phase, Standby; dissolve 200mg of crude stilbene glycosides in 10mL of the lower layer solution, and set aside;

[0034] (2) Use semi-preparative high-speed countercurrent chromatograph, with the ternary solvent system that above-mentioned ethyl acetate, ethanol and water form as separation solvent system; In the chromatographic column of high-speed countercurrent chromatograph, be full of stationary phase, then adjust rotating speed 900r / Min to make the host rotate, set the temperature of the constant temperature water bath to 25°C, set the detection wavelength of the ultraviolet detector to 280nm, then pump the mobile phase into the chromatographic column at 2mL / min; Styrene glycoside crude product (injection for the second time wh...

Embodiment 3

[0036](1) Mix ethyl acetate, ethanol and water at a volume ratio of 50:1:50, place in a separatory funnel, shake fully and leave to separate layers, take the upper layer solution as the stationary phase, and the lower layer solution as the mobile phase, Standby; dissolve 400mg of crude stilbene glycosides in 20mL of the lower layer solution to prepare a crude sample, and set aside;

[0037] (2) Use semi-preparative high-speed countercurrent chromatograph, with the ternary solvent system that above-mentioned ethyl acetate, ethanol and water are formed as separation solvent system; In the chromatographic column of high-speed countercurrent chromatograph, be full of stationary phase, then adjust rotating speed 950r / Min to make the host rotate, set the temperature of the constant temperature water bath to 25°C, set the detection wavelength of the ultraviolet detector to 280nm, and then pump the mobile phase into the chromatographic column at 3mL / min; Crude styrene glycosides, rec...

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Abstract

The invention provides a method for separating and purifying stilbene glucoside monomers, which adopts high-speed counter-current chromatography and uses a ternary solvent system composed of ethyl acetate, ethanol and water as a separation solvent system to separate and extract the stilbene glucoside monomers from a crude stilbene glucoside product. The separating and purifying method of the invention adopts a semi-preparative high-speed counter-current chromatograph to separate and purify the crude stilbene glucoside product, allows the crude stilbene glucoside product to go through the ternary solvent system, and utilizes the characteristics of high recovery rate and no irreversible adsorption of the high-speed counter-current chromatography to massively prepare the stilbene glucoside monomers, and the preparation amount can reach a gram magnitude; and the purity of the prepared stilbene glucoside monomers, which is high, reaches above 99%, and a standard sample of the stilbene glucoside monomers can be prepared with the high purity stilbene glucoside monomers as a raw material. The method of the invention is suitable for different crude stilbene glucoside products, and has the advantages of advanced technology, high separation efficiency, good recovery rate, high product purity, large preparation amount and the like.

Description

technical field [0001] The invention relates to a method for separating and purifying stilbene glycoside monomers, in particular to a method for separating and purifying stilbene glycoside monomers by high-speed countercurrent chromatography. Background technique [0002] Modern medicine has shown that Polygonum multiflorum has many functions such as enhancing immune function, anti-oxidation, delaying brain aging, improving DNA repair function, prolonging life, lowering cholesterol, and improving fat metabolism. The main components of Radix Polygoni Multiflori are hydroxyanthraquinone compounds (mainly emodin, chrysophanol, rhein and other glucosides, all of which are stilbene compounds), quinone compounds, stilbene glycoside compounds, amide compounds, color Protoketones, lecithin, and trace elements calcium, iron, zinc, manganese, copper, etc. Among them, stilbene glycoside is a unique bioactive component in Polygonum multiflorum, which has good water solubility and has m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/203C07H1/06
Inventor 王尉王覃张经华周晓晶赵新颖刘清珺武会娟
Owner BEIJING CENT FOR PHYSICAL & CHEM ANALYSIS
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