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Separation and purification method of populus diversifolia glucoside A and B monomers

A technology for separation and purification of monomers, which is applied in the field of separation and purification of myricin A and B monomers

Inactive Publication Date: 2021-03-12
GUANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the problem that there is no separation and purification of myricin monomers at present, the present invention provides a method for separation and purification of myricin A and B monomers

Method used

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  • Separation and purification method of populus diversifolia glucoside A and B monomers
  • Separation and purification method of populus diversifolia glucoside A and B monomers
  • Separation and purification method of populus diversifolia glucoside A and B monomers

Examples

Experimental program
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Effect test

Embodiment 1

[0035] A method for separating and purifying miyanin A and B monomers, comprising the steps of:

[0036] 1) Take 10 kg of dried Mi Yang leaves, add 10 times the raw material mass ratio of 65% ethanol aqueous solution (volume ratio), heat and reflux for extraction 3 times in sequence, the time is 3 hours, 2 hours, and 2 hours, combine the filtrates, and recover ethanol under reduced pressure , get extract;

[0037] 2) Dilute the extract of step 1) 50 times with distilled water, absorb it on a D101 macroporous adsorption resin chromatographic column, wash and rinse with 4 column volumes of distilled water to remove unadsorbed impurities, and then use each 4 column volumes of Elution with 10% ethanol aqueous solution and 30% ethanol aqueous solution, discard the eluent, then elute with 40% ethanol aqueous solution, concentrate the eluent to obtain the eluted fraction rich in myricin A and B;

[0038] 3) Take the 40% ethanol eluate obtained in step 2), and through silica gel colu...

Embodiment 2

[0049] A method for separating and purifying miyanin A and B monomers, comprising the steps of:

[0050] 1) Get 10kg of dried Mi Yang leaves, add 12 times of 73% ethanol aqueous solution (mass ratio of raw materials), heat and reflux and extract 3 times successively, the time is 3 hours, 2 hours, 2 hours, combine the filtrates, reclaim ethanol under reduced pressure, and obtain extract;

[0051] 2) Take the extract and suspend it in 50L of water, absorb it through a D101 macroporous adsorption resin chromatographic column, wash it with water, and then elute it with 20% and 50% ethanol to obtain 20%, 50% ethanol eluate and 50% ethanol eluate respectively. The detoxification is used as the extract of Mi Yang choke leaf which is rich in Mi Yang glycosides A and B;

[0052] 3) Take 625.0 g of the 50% ethanol eluate obtained in the above step 2), through silica gel column chromatography, use 4 column volumes of 4% dichloromethane and 96% methanol mixed solution, 10% Mixed solutio...

Embodiment 3

[0057] A method for separating and purifying miyanin A and B monomers, comprising the steps of:

[0058] 1) Get 10kg of dried Mi Yang leaves, add 15 times of 75% ethanol aqueous solution (mass ratio of raw materials), heat and reflux and extract 3 times successively, the time is 3 hours, 2 hours, 2 hours, combine the filtrates, reclaim ethanol under reduced pressure, and obtain extract;

[0059] 2) Suspend the medicinal extract of step 1) in 50L of water, absorb on a D101 macroporous adsorption resin chromatographic column, wash with water, and then elute with 20% and 50% ethanol to obtain 20% and 50% ethanol eluates respectively, The 50% ethanol eluate is used as the extract of Mi Yang choke leaf which is rich in mi Yang glucosides A and B;

[0060] 3) Take the 50% ethanol eluate obtained in the above step 2), and through silica gel column chromatography, use 4 column volumes of 5% dichloromethane and 95% methanol mixed solution, 10% dichloromethane Chloromethane and 90% me...

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Abstract

The invention discloses a separation and purification method of populus miyabensis choking glycoside A and B monomers, and the method comprises the following steps: by using populus miyabensis chokingleaves as a raw material, extracting with ethanol with specific concentration, adsorbing with macroporous adsorption resin, carrying out silica gel chromatographic column chromatography, and finallypurifying with a high performance liquid chromatography C18 silica gel chromatographic column to obtain two new monomer compounds. The method can effectively remove a large amount of impurities in thepopulus miyunnanensis dysphagia, two populus miyunnanensis dysphagia glycosides can be obtained at a time, and therefore a material basis can be provided for activity research of populus miyunnanensis dysphagia glycosides compounds and development of new drugs with a single component.

Description

technical field [0001] The invention relates to the technical field of separation and purification of active ingredients of traditional Chinese medicines, in particular to a method for separation and purification of myricin A and B monomers. Background technique [0002] Streblus tonkinensis belongs to the genus Strebluslour. in the family Moraceae. The genus Streblus lour. belongs to the Moraceae family of plants. Mi Yang is often used as a folk medicinal plant to treat diseases. According to the literature research, so far there is no report on the chemical constituents and biological activities of Mi Yang choke. Based on the fact that Mi Yang is a commonly used medicinal plant in the folk, in order to better study the ingredients in it, develop and utilize the plant, and find a better extraction rate, low cost and easy industrial production of Mi Yang Yan A and The separation and purification process of B can lay the foundation for the study of the characteristic biolo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/18C07H1/08
CPCC07B2200/07C07H1/08C07H15/18
Inventor 李俊张高荣周德雄黄锡山黄艳邓胜平
Owner GUANGXI NORMAL UNIV
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