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Method for separating flavone monomers from spina gleditsiae based on counter-current chromatography

A technology of countercurrent chromatography and stabbing flavonoids, which is applied in the field of flavonoid monomer compound extraction, can solve the problems of low recovery rate, long separation cycle, unsatisfactory separation effect, etc., and achieve the effect of simple operation and good stability

Active Publication Date: 2020-09-29
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this method are: long separation period, low recovery rate, and unsatisfactory separation effect. When using silica gel column chromatography and reversed-phase column chromatography, the structure of this type of component will occur due to contact with silica gel and reversed-phase C18 packing for a long time. Variety

Method used

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  • Method for separating flavone monomers from spina gleditsiae based on counter-current chromatography
  • Method for separating flavone monomers from spina gleditsiae based on counter-current chromatography
  • Method for separating flavone monomers from spina gleditsiae based on counter-current chromatography

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Embodiment 1

[0041] In this embodiment, a method for separating and purifying flavonoid monomers from Saponaria thorn based on high-speed countercurrent chromatography is provided, and the method includes the following steps:

[0042] Take the saponin root medicinal material, crush it to 40-60 mesh, heat and reflux extraction with 95% ethanol, the solid-to-liquid ratio is 1:3, extract three times for 2 hours, 1 hour, and 1 hour respectively, combine the filtrates, spin-evaporate under reduced pressure, and freeze-dry , to obtain the crude extract of Saponaria thorn; the crude extract in step 1 is dispersed with water, extracted with petroleum ether and ethyl acetate respectively, and the extract is concentrated under reduced pressure to obtain petroleum ether, ethyl acetate and water parts respectively, wherein the acetic acid The ethyl ester part is mainly flavonoids, the liquid phase analysis diagram is shown in figure 2 .

[0043] Apply high-speed countercurrent chromatography to the ...

Embodiment 2

[0056] In the present embodiment, a method for separating and purifying flavonoid monomers from Saponaria thorn based on countercurrent chromatography is provided, and the method includes the following steps:

[0057] (1) Preparation of saponinsia thorn extract: take saponinsia thorn medicinal material, pulverize, extract under reflux with 90% ethanol, the solid-to-liquid ratio is 1:4, extract four times, the time is 2h, 1h, 1h, 1h respectively, and combine The filtrate was rotary evaporated under reduced pressure, and freeze-dried to obtain the crude extract of Saponaria japonica;

[0058] (2) Disperse the crude extract in step 1 with water, extract with petroleum ether and ethyl acetate respectively, and concentrate under reduced pressure to obtain petroleum ether, ethyl acetate and water part concentrate;

[0059] (3) Separation of the monomer: the solvent system is methylene chloride: methanol: n-butanol: water=4:3:0.5:2 (v / v), the upper phase is the stationary phase, the ...

Embodiment 3

[0062] In the present embodiment, a method for separating and purifying flavonoid monomers from Saponaria thorn based on countercurrent chromatography is provided, and the method includes the following steps:

[0063] (1) Preparation of the saponins thorn extract: Take the saponinsia thorns medicinal material, pulverize, heat and reflux extraction with 98% ethanol, the solid-to-liquid ratio is 1:2, extract twice for 3 hours and 2 hours respectively, combine the filtrates, and decompress Rotary steaming, freeze-drying to obtain the crude extract of Saponaria thorn;

[0064] (2) Disperse the crude extract in step 1 with water, extract with petroleum ether and ethyl acetate respectively, and concentrate under reduced pressure to obtain petroleum ether, ethyl acetate and water part concentrate;

[0065] (3) Separation of the monomer: the solvent system is methylene chloride: methanol: n-butanol: water=4:3:0.5:2 (v / v), the upper phase is the stationary phase, the lower phase is the...

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Abstract

The invention particularly relates to a method for separating flavonoid monomers in spina gleditsiae based on counter-current chromatography. Existing researches prove that flavonoid components in thespina gleditsiae have good anti-tumor and antioxidant activity. The invention aims to extract and separate high-value flavone monomers in spina gleditsiae. And a method for producing the same. The invention, based on said purpose, provides a method for separating flavonoid monomers from spina gleditsiae based on counter-current chromatography, which comprises the following steps: preparing an ethanol extract of spina gleditsiae, sequentially extracting the ethanol extract by using petroleum ether and ethyl acetate, separating the ethyl acetate extract by counter-current chromatography, and finally carrying out chromatographic separation to obtain five flavonoid monomers. The method overcomes the defects of complex operation, dead adsorption loss of the sample, low yield and the like of the traditional preparation methods. The method is high in efficiency, simple to operate and low in comprehensive cost, and has good popularization and use values.

Description

technical field [0001] The invention belongs to the technical field of extraction of flavonoid monomer compounds, and in particular relates to a method for separating flavonoid monomers from saponins root based on high-speed countercurrent chromatography. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Gleditsiae Spina, also known as Gleditsiae Spina, Gleditsiae Spina, etc., is the dry thorn of Gleditsia sinensis Lam. in the family Leguminosae, and is a traditional Chinese medicinal material. , has a long history of clinical application and extensive medicinal value. It is pungent in taste, warm in nature, and returns to the liver and stomach meridians. It has the effect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/40C07H1/08C07H17/07
CPCC07D311/40C07H1/08C07H17/07
Inventor 于金倩王晓王岱杰耿岩玲孙成龙
Owner SHANDONG ANALYSIS & TEST CENT