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Method for efficiently separating and purifying forsythiaside B monomer and poliumoside monomer

A technology of chrysanthiside and forsythiaside, which is applied in the field of high-efficiency separation and purification of forsythiaside B and chrysanthiside monomers, and can solve the problem of preparation and separation of forsythiaside B and nymphin monomers that have not been reported , There are no problems such as forsythiaside B and chrysanthaside gram-grade products, difficulty in separating monomers, etc., and achieve the effects of easy quality control, large output, and efficient process

Inactive Publication Date: 2012-11-07
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, Forsythiaside B and Chrysoside have been listed as standards in the 2010 Pharmacopoeia, and the demand for these two monomers is increasing, especially the content of Chrysoside in medicinal materials is very low. It is very difficult to separate the monomers, and there is no gram-grade product of forsythiaside B and silgoside in the market at present, and there is no report on the preparation and separation of forsythiaside B and silgoside monomers. Therefore, from Guangdong It is very necessary to separate and purify forsythiaside B and shicroside monomers from purple pearls, and has wide application value

Method used

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  • Method for efficiently separating and purifying forsythiaside B monomer and poliumoside monomer
  • Method for efficiently separating and purifying forsythiaside B monomer and poliumoside monomer
  • Method for efficiently separating and purifying forsythiaside B monomer and poliumoside monomer

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Experimental program
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Effect test

Embodiment 1

[0027] A high-efficiency separation and purification method for forsythiaside B and shicroside monomer, characterized in that it is carried out according to the following process steps:

[0028] a. Extraction and concentration of Guangdong Zizhu medicinal material: take 10kg of Guangdong Zizhu medicinal material, crush it into 50 mesh powder, add 5 times the weight of the medicinal material in an ethanol solution with a concentration of 30% by volume, and reflux extraction at 60°C for 3 times, each time for 2h , combined the three extracts; recovered ethanol under reduced pressure at 70°C, concentrated to an aqueous solution, and filtered to obtain a concentrated solution;

[0029] b. Enrichment of Forsythiaside B and Chryserin: Adsorb the activated AB-8 macroporous resin on the concentrated solution obtained in step a. After the adsorption is complete, first elute with 3 times the column volume of water to remove the sugar Such large polar impurities are then analyzed with 3 ...

Embodiment 2

[0036] A high-efficiency separation and purification method for forsythiaside B and shicroside monomer, characterized in that it is carried out according to the following process steps:

[0037] a. Extraction and concentration of Guangdong Zizhu medicinal material: Take 5 kg of Guangdong Zizhu medicinal material, grind it into 60 mesh powder, add 5 times the weight of ethanol solution with a volume percentage concentration of 40%, and reflux extraction at 55 ° C for 3 times, each time for 2 hours, Combine the three extracts; recover ethanol under reduced pressure at 70°C, concentrate to an aqueous solution, and filter to obtain a concentrate;

[0038] b. Enrichment of Forsythiaside B and Chryserin: Adsorb the activated AB-8 macroporous resin on the concentrated solution obtained in step a. After the adsorption is complete, first elute with 3 times the column volume of water to remove the sugar Such large polar impurities are then analyzed with 3 times the column volume of 30% (V...

Embodiment 3

[0044] A high-efficiency separation and purification method for forsythiaside B and shicroside monomer, characterized in that it is carried out according to the following process steps:

[0045] a. Extraction and concentration of Guangdong Zizhu medicinal material: take 20kg of Guangdong Zizhu medicinal material, crush it into 40 mesh powder, add 8 times the weight of ethanol solution with a volume percentage concentration of 50%, and reflux extraction at 65°C for 3 times, each time for 2h, Combine the three extracts; recover ethanol under reduced pressure at 80°C, concentrate to an aqueous solution, and filter to obtain a concentrate;

[0046] b. Enrichment of Forsythiaside B and Chryserin: Adsorb the activated AB-8 macroporous resin on the concentrated solution obtained in step a. After the adsorption is complete, first elute with 3 times the column volume of water to remove the sugar Such large polar impurities are then analyzed with 3 times the column volume of 30% (V / V) e...

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Abstract

The invention discloses a method for efficiently separating and purifying a forsythiaside B monomer and a poliumoside monomer, comprising the following steps: extracting extract from ground herbal medicine of callicarpa kwangtungensis Chun as a raw material by using polar solvent, enriching by using AB-8 macroporous resin, removing sugar and other large polar impurities, decolorizing by the silica gel column chromatography, carrying out rough separating, separating and purifying semi-finished product obtained after rough separating by the preparative high performance liquid chromatography column, detecting in an on-line manner by using a differential refraction detector, pertinently collecting forsythiaside B monomer solution and poliumoside monomer solution, and respectively processing and drying the forsythiaside B monomer solution and the poliumoside monomer solution to obtain the forsythiaside B monomer and the poliumoside monomer with the purity more than 98 percent. According tothe invention, the synchronous separation of the forsythiaside B and the poliumoside can be realized; and the method provided by the invention has the advantages of large preparation quantity, high yield and good product quality, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for separating and purifying monomer active components in plants, which belongs to the technical field of medicine. Specifically, the invention relates to a method for isolating high-purity forsythiaside B and silcroside monomers from Guangdong Zizhu medicinal materials The method, and the high performance liquid chromatography analysis method of forsythiaside B and silicoside monomer. Background technique [0002] Guangdong Zizhu (Callicarpa kwangtungensis Chun.) is a plant of the genus Callicarpa L. in the Verbenaceae (Verbenaceae). Fujian, Hubei, Hunan, Guangdong, Guangxi, Guizhou, Yunnan and other places, recorded in Jiangxi Provincial Standards of Medicinal Materials (1996 edition, page 24), its medicinal parts are dried stems, branches and leaves, which have the functions of astringent, hemostatic, heat-clearing and detoxifying effect. For hemoptysis, epistaxis, hematochezia, lung and stomach bleeding, metrorrh...

Claims

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Application Information

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IPC IPC(8): C07H15/18C07H1/08
Inventor 常建红郭建华刘丁
Owner CHENGDU PUSH BIOLOGICAL TECH