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Method for synchronously separating liquiritin and liquiritin apioside from liquorice

A technology of glycyrrhizin apiose and synchronous separation, which is applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc. Complex chemical composition and other problems, to achieve the effect of fast adsorption, easy industrial amplification, and high mechanical strength

Active Publication Date: 2015-07-01
YANTAI INST OF COASTAL ZONE RES CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, there are many methods for separating and purifying active ingredients, mainly chromatography, but there are great differences in the types and structures of active ingredients contained in different plants, so there are differences in chemical properties. General methods are used in the extraction and purification process. In the extraction and purification method, the purity of the active ingredient obtained is not high. If a high purity is to be achieved, the separation efficiency is low and the cost is high
At present, there are few reports on the extraction and purification of high-purity liquiritin and liquiritin-galloside from licorice, and the chemical components in licorice are complex, which is very difficult in the extraction and separation process
The publication number is CN101289480, and the invention name is a patent for the separation and preparation method of liquiritin, in which the patent uses water extraction, alcohol precipitation, membrane separation, and then uses macroporous resin to separate liquiritin; the publication number is CN102050851A, and the invention name is liquiritin and its preparation method The patent is to extract liquiritin from glycyrrhizic acid powder, extract it with dilute ammonia water, extract it with organic solvent, and then separate it with polyamide resin; the publication number is CN102391330A, and the invention name is the patent of the method of extracting liquiritin from licorice. , over-mixed resin column separation to obtain liquiritin, but these methods all adopt the single-stage separation mode, and the yield is low, so it is not suitable for large-scale production; the application number is 200710011041.0 Invention name A kind of preparation method of liquiritin discloses that the licorice medicinal material is passed through water Extraction, alcohol precipitation, separation by molecular weight membrane separator, macroporous resin column, and high-efficiency industrial chromatographic column, and freeze-drying to obtain liquiritin. Although this method has a large amount of preparation at one time, the method still adopts a single-stage separation method, and the production efficiency is high. low, and only obtained liquiritin, resulting in a waste of resources
[0004] In short, the existing methods all have the disadvantages of intermittent and discontinuous operation, low utilization rate of upper column liquid and eluent, etc. Reasonable use of the advantages of selective adsorption separation of resin and optimization of separation process will greatly reduce production costs and improve production Efficiency, non-toxic and environmental protection, open up a new industrial pattern for the preparation process of liquiritin and liquiritin celulose

Method used

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  • Method for synchronously separating liquiritin and liquiritin apioside from liquorice
  • Method for synchronously separating liquiritin and liquiritin apioside from liquorice
  • Method for synchronously separating liquiritin and liquiritin apioside from liquorice

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) Extraction: Take 0.5kg of licorice powder, add 5L of methanol with a volume fraction of 85%, heat and reflux for extraction for 2 hours, filter, add 5L of 85% methanol to the filter residue, heat and reflux for 2 hours, filter, and combine the two extracts , extraction and hydraulic concentration to recycle the organic solvent, add water to the raffinate, and mix well to make the raffinate concentration 10g / L to obtain the intermediate product A.

[0036] (2) Primary separation and purification of the resin column: the intermediate product A passes through the D101 resin column filled with 3-stage serial series treated according to the conventional method at a flow rate of 3BV / h, and is dynamically adsorbed to breakthrough, wherein each stage of the D101 resin column The diameter-to-height ratio is 1:10; the resin column is eluted with water with a flow rate of 8BV / h to remove water-soluble impurities, and the water analysis solution is discarded; the tandem resin co...

Embodiment 2

[0042] (1) Extraction: Take 1kg of licorice powder, add 10L of 75% methanol, extract by ultrasonic for 2h, filter, add 10L of 75% methanol to the filter residue, extract by ultrasonic for 2h, filter, combine the two extracts, and decompress the extract Concentrate and recover the organic solvent, add water to the raffinate, and mix well to make the concentration 8g / L, and then intermediate product A is obtained.

[0043] (2) Primary separation and purification of the resin column: the intermediate product A passes through the AB-8 resin column filled with a diameter-to-height ratio of 1:8 at a flow rate of 5BV / h, 4 stages are connected in series, and are dynamically adsorbed to breakthrough. The diameter-to-height ratio of the AB-8 resin column is 1:6; the resin column is eluted with water with a flow rate of 8BV / h to remove water-soluble impurities, and the water analysis solution is discarded; wash with 70% ethanol at a speed of 5BV / h The tandem resin column after impurity i...

Embodiment 3

[0047] (1) Extraction: Take 2kg of licorice powder, add 20L of 70% ethanol, extract by ultrasonic for 1h, filter, add 20L of 70% ethanol to the filter residue, ultrasonically for 1h, filter, combine the two extracts, and concentrate the extract under reduced pressure Recover the organic solvent, add water to the raffinate, and mix well to make the concentration 12g / L to obtain the intermediate product A.

[0048] (2) Primary separation and purification of the resin column: the intermediate product A passes through the D101 resin column filled with the conventional method at a flow rate of 8BV / h, 5 stages in series, the diameter-to-height ratio is 1:10, and is dynamically adsorbed to breakthrough , the resin column was eluted with water at a flow rate of 10BV / h to remove water-soluble impurities, and the water analysis solution was discarded. Use 60% ethanol to elute the tandem resin column after washing at 6BV / h, collect the eluate until the eluate is colorless, concentrate th...

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Abstract

The invention relates to a method for preparing active ingredients from Chinese medicinal herbs, in particular to a method for synchronously separating liquiritin and liquiritin apioside from liquorice. The method comprises the steps of taking the liquorice as a raw material, conducting heating reflux or ultrasonic extraction, macroporous resin series adsorption and gradient desorption, then conducting secondary adsorption and desorption after recovering organic solvent from an analytic solution, and finally obtaining the liquiritin and the liquiritin apioside simultaneously with purities of 90%-98% through a medium-pressure gradient elution system. The method is short in process flow, simple to operate and low in cost, can simultaneously separate the high-purity liquiritin and liquiritin apioside, and is applicable to larger-scale preparation.

Description

technical field [0001] The invention relates to a method for preparing active ingredients from Chinese herbal medicines, in particular to a method for synchronously separating liquiritin and liquiritin celery from licorice. Background technique [0002] Licorice is a leguminous plant Glycyrrhiza uralensis Fisch. , Glycyrrhiza inflata Bat. Or Glycyrrhiza glabra L. dry roots and rhizomes. Clinical applications include licorice and roasted licorice. Among them, licorice has the functions of invigorating the spleen and replenishing qi, clearing away heat and detoxification, reducing phlegm and relieving cough, relieving spasm and relieving pain, etc. Licorice mainly contains saponins and flavonoids. Studies have found that licorice flavonoids have antibacterial, anti-oxidant, anti-tumor, anti-viral and other physiological activities. Liquiritin is the main flavonoid component in licorice, which has antiviral, antioxidative and antiarrhythmic effects. At the same time, liqui...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/26C07H1/08
Inventor 夏传海孔娜娜方圣涛刘霞王建华
Owner YANTAI INST OF COASTAL ZONE RES CHINESE ACAD OF SCI
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