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A kind of separation and purification method of dandelion total flavonoids

A technology for separation and purification of total flavonoids, applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., can solve the problems of poor overall economic benefits, high chromatographic costs, and large consumption of pretreatment reagents, etc., to achieve production costs Low cost, rich source of raw materials, good adsorption selectivity

Inactive Publication Date: 2016-08-10
DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent application with the publication number CN10198218IA discloses a preparation method of dandelion extract, the product content is as high as more than 90%, but the extraction and separation process consumes a lot of resin pretreatment reagents, and the chromatographic cost in the later stage of refining is relatively high. The overall economic benefit is far inferior to the separation and purification method involved in this patent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take by weighing 10 kg of the whole dandelion herb, crush it into a coarse powder, add 18 times the amount of 90% methanol for reflux extraction for 140 minutes, and filter; The pH value of the concentrated solution was adjusted to 2.8, left to stand for 40 minutes, and filtered; the filtrate was placed on a HPD100 type macroporous resin adsorption column, and the impurities were washed with water after adsorption, and then washed with 15% methanol, and then eluted with 70% methanol to obtain Total flavonoid semi-finished product eluate, total flavonoid semi-finished product eluent reclaims methanol and concentrates and dries to obtain total flavonoid semi-finished product; Gained total flavonoid semi-finished product is put on silica gel chromatography column, and the volume ratio of acetone:methanol is 2: 1 mixture of acetone and methanol Wash the impurities, then elute with a mixture of acetone and methanol with a volume ratio of acetone:methanol of 6:1 to obtain 2L o...

Embodiment 2

[0022] Take by weighing 15 kg of whole dandelion herb, crush it into a coarse powder, add 20 times the amount of 95% methanol for reflux extraction for 160 minutes, and filter; The pH value of the concentrated solution was adjusted to 3, left to stand for 40 minutes, and filtered; the filtrate was placed on a HPD400 type macroporous resin adsorption column, and the impurities were washed with water after adsorption, and then washed with 10% methanol, and then eluted with 60% methanol to obtain Total flavonoid semi-finished product eluent, total flavonoid semi-finished product eluent reclaims methanol, concentrates and dries to obtain total flavonoid semi-finished product; puts the obtained total flavonoid semi-finished product on a silica gel chromatography column, and uses acetone:methanol volume ratio as 1: 1 mixture of acetone and methanol Wash the impurities, and then use acetone:methanol to elute with a mixture of propanol and methanol with a volume ratio of 7:1 to obtain ...

Embodiment 3

[0024] Take by weighing 20kg of the whole dandelion herb, crush it into a coarse powder, add 15 times the amount of 87% methanol to reflux and extract for 120 minutes, and filter; Adjust the pH value of the concentrated solution to 2.5, let it stand for 40 minutes, and filter; put the filtrate on an AB-8 macroporous resin adsorption column, wash the impurities with water after adsorption, then wash the impurities with 5% methanol, and then elute with 80% methanol , to obtain the total flavonoids semi-finished product eluent, the total flavones semi-finished product eluent reclaims methanol and concentrates and dries to obtain the total flavones semi-finished product; the gained total flavonoids semi-finished product is put on a silica gel chromatography column, and the volume ratio of acetone: methanol is 3: 1 with acetone and Methanol mixture was used to wash impurities, and then eluted with a mixture of acetone and methanol with a volume ratio of acetone:methanol of 5:1 to ob...

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Abstract

The invention discloses a method for separating and purifying total flavone of dandelion. The method comprises the following steps: whole dandelion is shattered into coarse powder, added with methanol (85 percent) which is 15 times of the whole dandelion in quantity, refluxed and extracted for 120 minutes, and filtered; a filtrate recovers the methanol and is concentrated to 3 beaume, the pH value of a concentrate is regulated to 2.5 by hydrochloric acid and water which are 1:1 in volume ratio, and the concentrate is placed for 20 minutes and filtered; the filtrate is loaded on a broad-spectrum macroporous resin adsorbent column, collects an eluant, recovers the methanol, and is concentrated and dried to obtain the semi-product of the total flavone; the obtained semi-product of the total flavone is loaded on a silica gel chromatography column, of which impurities are removed by acetone and the methanol which are 3:1 in volume ratio, and is continuously eluted by the acetone and the methanol which are 7:1 in volume ratio, and the eluant is collected; the collected eluant of the total flavone is refined to obtain the finished product of the total flavone of which content is over 96 percent. The method is mainly characterized in that the utilized macroporous polymeric adsorbent-silica gel chromatography and coupling method is convenient and quick; the sources of raw materials are abundant; the production cost is low; the separation effect is remarkable; and the extract purity is high.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry, and relates to a method for separating and purifying total flavonoids of dandelion, in particular to a method for enriching and purifying total flavonoids of dandelion by using a macroporous adsorption resin-silica gel chromatography coupling method. Background technique: [0002] Dandelion, also known as bed-wetting grass, is Toraxacum mongolicum Hand.Mazz. and Toraxacum borealisinense Kitam. Or dry whole grass of several plants of the same genus. The whole herb is used as medicine, and the roots are collected before flowering, washed and dried in the sun. Dandelion contains a variety of active ingredients, such as dandelion sterols, dandelion bitters, flavonoids, caffeic acid, chlorogenic acid and polysaccharides. [0003] The total flavonoids of dandelion have the functions of clearing heat and detoxifying, reducing swelling and dissipating stagnation, diuresis and treating strangur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K36/288B01D15/10A61P31/00A61P29/00A61P7/10A61P15/14A61P31/06A61P17/00A61P11/04A61P11/00A61P1/00A61P27/02A61P13/00A23L33/00
Inventor 姚德坤姚德利张亚红姚航黄运生吴海龙
Owner DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD