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Method of dual-aqueous phase system for purifying polygala root xanthonoid compound

A two-phase system and xanthone technology, which is applied in the field of natural plant extraction and purification, can solve the problems of enrichment and separation of polygala xanthone compounds that have not been seen in two-phase systems, and achieve shortened production cycles and easy recycling , the effect of simple operation

Inactive Publication Date: 2011-11-02
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Existing methods for extraction, enrichment and separation of xanthone compounds mainly include solvent extraction, organic solvent extraction, column chromatography, etc., and there is no report on the enrichment and separation of xanthanone compounds by using a two-phase system

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Preparation of Polygala extract: Pulverize Polygala root into coarse powder, take 5 kg and use 60% ethanol as extraction solvent with a solid-to-liquid ratio of 1:8, ultrasonically extract for 40 minutes, extract twice, and combine the extracts.

[0024] (2) Macroporous resin adsorption: Concentrate the extract to obtain ethanol extract, dissolve it with an equal volume of distilled water, place it on a D101 macroporous adsorption resin column, wash it with distilled water until the effluent is colorless, and then wash it with 4 times the column The ethanol with 50% of the bed volume was eluted, the ethanol eluate was collected, and the ethanol was recovered under reduced pressure to 1 / 5 of the original volume to obtain a concentrated solution.

[0025] (3) two-phase extraction: take the concentrated solution and add ammonium sulfate and ethanol to mix evenly, so that the volume ratio of the concentrated solution to ethanol is 3:1, the mass concentration of ammonium ...

Embodiment 2

[0029] (1) Preparation of polygala extract: Pulverize polygala root into coarse powder, take 5 kg and use 70% ethanol as the extraction solvent with a solid-to-liquid ratio of 1:10, ultrasonically extract for 30 minutes, extract twice, and combine the extracts.

[0030] (2) Macroporous resin adsorption: Concentrate the extract to obtain ethanol extract, dissolve it with distilled water of equal volume, place it on the AB-8 macroporous adsorption resin column, wash it with distilled water until the effluent is colorless, and then wash it with 5 The column bed volume was eluted with 65% ethanol, the ethanol eluate was collected, and the ethanol was recovered under reduced pressure to 1 / 6 of the original volume to obtain a concentrated solution.

[0031] (3) Two-phase extraction: get the concentrated solution and add ammonium sulfate and ethanol to mix evenly, so that the volume ratio of the concentrated solution to ethanol is 3:1, the mass concentration of ammonium sulfate is 20%...

Embodiment 3

[0035] (1) Preparation of polygala extract: Pulverize polygala root into coarse powder, take 5 kg and use 90% ethanol as extraction solvent with a solid-to-liquid ratio of 1:6, ultrasonically extract for 50 minutes, extract twice, and combine the extracts.

[0036] (2) Macroporous resin adsorption: Concentrate the extract to obtain ethanol extract, dissolve it with an equal volume of distilled water, place it on a HPD100 macroporous adsorption resin column, wash it with distilled water until the effluent is colorless, and then wash it with 3 times the column The ethanol of 60% of the bed volume was eluted, and the ethanol eluate was collected, and the ethanol was recovered under reduced pressure to 1 / 8 of the original volume to obtain a concentrated solution.

[0037] (3) Two-phase extraction: get the concentrated solution and add ammonium sulfate and ethanol to mix evenly, so that the volume ratio of the concentrated solution to ethanol is 3:1, the mass concentration of ammoni...

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PUM

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Abstract

The invention relates to a method of a dual-aqueous phase system for purifying a polygala root xanthonoid compound. The method comprises the following steps: performing an ultrasonic sound of polygala root by using 60% to 90% of ethanol or performing a reflux extraction by heating, and then filtering and concentrating, performing a macroporous adsorption resin column on a concentrate, eluting with 50% to 65% of ethanol, concentrating an eluate and then adding ammonium sulfate and the ethanol dual-aqueous phase system according to a proportion, heating and uniformly mixing to divide into an upper phase and a bottom phase; cooling the bottom phase and crystallizing to recovery ammonium sulfate crystals, taking the upper phase containing ethanol out and adding ethyl acetate, water and sodium chloride, uniformly mixing and taking the upper phase containing polygala root xanthonoid compound, reducing pressure and concentrating, performing a vacuum drying to obtain the polygala xanthonoid compound. According to the invention, the polygala root xanthonoid compound can be separated by a macroporous resin and purified by using a dual-aqueous phase extraction technology, which has simple operation and provides technical foundation to industrialization of the polygala root xanthonoid compound.

Description

Technical field: [0001] The invention belongs to the technical field of extraction and purification of natural plants, and relates to a method for purifying polygala xanthone compounds in a two-phase system. Background technique: [0002] Polygala is the dried root of Polygala tenuifolia Willd. and Polygala sibirica L., which are plants of the Polygalaceae family. It is mainly produced in Shanxi, Shaanxi, Henan, Inner Mongolia and other places. Insomnia, dreaminess, forgetfulness, palpitations, trance, coughing up phlegm, sore swelling, breast swelling and pain caused by heart-kidney disharmony. Its chemical composition mainly includes saponins, xanthones and sugar esters. Pharmacological studies have shown that xanthone ketones have a wide range of pharmacological activities, including diuretic, antimicrobial, antiviral, cardiotonic, antidepressant, antituberculosis, and anticancer activities. Most xanthones can inhibit monoamine oxidase A and B. Some xanthone compounds,...

Claims

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Application Information

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IPC IPC(8): C07D311/86
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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