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Method for extracting and separating effective part from dogbane

A technology of effective parts and separation methods, applied in the field of extraction and separation of effective parts of Apocynum apocynum, can solve problems such as unsuitable for industrial production, inability to use apocynum for separation, high toxicity, etc.

Inactive Publication Date: 2004-12-15
李青山
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the extraction methods of the effective parts of Apocynum apocynum mainly include water extraction and alcohol extraction. The separation method includes the preparation step of the column liquid on the apocynum apocynum, the separation step of the separation column composed of specific separation substances, and the separation with a specific eluent. The step of eluting the column and concentrating the eluent, etc., the above-mentioned separation column in the prior art adopts a silica gel column, because the silica gel column is used for separation and chromatography is basically a single-component substance, so the existing Technology can not be used for the separation of the effective part of Apocynum venetifolia, and the eluent used is basically organic solvent (as benzene, CHCl 3 etc.), the toxicity is relatively large, therefore, the existing extraction and separation methods are not suitable for industrial production, and are mainly used as a means of chemical composition research in Apocynum apocynum

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] 80 grams of Apocynum apocynum is extracted with 20 times of 60% ethanol aqueous solution for 2-4 times in reflux, each time for 30-90 minutes, the filtrates obtained each time are combined, after removing chlorophyll, they are concentrated to a certain volume as the upper column liquid.

[0011] Soak the macroporous adsorption resin in 95% ethanol solution for more than 4 hours, then wash it with 95% ethanol solution until the effluent is not turbid, and then wash it with distilled water until it has no alcohol smell and no turbidity.

[0012] Put the prepared loading solution directly on the column.

[0013] First, the macroporous adsorption resin column is eluted with water until the water eluent is colorless, then, eluted with 20% ethanol aqueous solution, FeCl can be used 3 The eluate was tested to prove that the tannin was eluted completely, when the eluate was mixed with FeCl 3 When the reaction does not show dark green, it proves that the tannin has been eluted ...

Embodiment 2

[0020] Take 80 grams of Apocynum apocynum, use 25 times of 40% ethanol aqueous solution to reflux extraction for 2-4 times, each time for 30-90 minutes, combine the filtrates obtained each time, after removing chlorophyll, concentrate to a certain volume as the upper column liquid .

[0021] Soak the macroporous adsorption resin in 95% ethanol solution for more than 4 hours, then wash it with 95% ethanol solution until the effluent is not turbid, and then wash it with distilled water until it has no alcohol smell and no turbidity.

[0022] Mix the prepared loading solution with an appropriate amount of macroporous adsorption resin, dry it and put it on the column directly, and let it stand for 12 hours.

[0023] First, the macroporous adsorption resin column is eluted with water until the water eluent is colorless, then, eluted with 30% ethanol aqueous solution, FeCl can be used 3 The eluate was tested to prove that the tannin was eluted completely, when the eluate was mixed ...

Embodiment 3

[0030] Take 80 grams of Apocynum apocynum, use 15 times of 70% ethanol aqueous solution to reflux extraction for 2-4 times, each time for 30-90 minutes, combine the filtrates obtained each time, remove the chlorophyll, concentrate to a certain volume as the upper column liquid .

[0031] Soak the macroporous adsorption resin in 95% ethanol solution for more than 4 hours, then wash it with 95% ethanol solution until the cleaning effluent is not turbid, and then wash it with distilled water until it has no alcohol smell and no turbidity.

[0032] Put the prepared loading solution directly on the column.

[0033] First use 35% ethanol aqueous solution to elute the macroporous adsorption resin column, FeCl can be used 3 The eluate was tested to prove that the tannin was eluted completely, when the eluate was mixed with FeCl 3 When the reaction does not show dark green, it proves that the tannin has been eluted completely, and then eluted with 70% ethanol aqueous solution until t...

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Abstract

The extraction and separation method of effective component of dogbane includes the following steps: loading dogbane liquor into chromatographic column, making separation by separation column, eluting separation column and concentrating eluent. Its separation column adopts macroporous adsorption resin column, and the elution step adopts 20-39% ethyl alcohol solution to make elution firstly, then uses 40-70% ethyl alcohal aqueous solution to make elution or uses water to make elution, then the eluent is concentrated to obtain the dogbane extract whose total flavone content is up to above 50%. The eluting agent used by said invention is non-toxic, and it is applicable to industrial poduction.

Description

technical field [0001] The invention relates to a method for extracting and separating effective parts of Chinese herbal medicines, in particular to a method for extracting and separating effective parts of apocynum. Background technique [0002] Apocynum apocynum is a kind of Chinese herbal medicine that has obvious curative effects on hypertension, hyperlipidemia, etc., and its effective part is the flavonoid compound contained in it. At present, the extraction methods of the effective parts of Apocynum apocynum mainly include water extraction and alcohol extraction. The separation method includes the preparation step of the column liquid on the apocynum apocynum, the separation step of the separation column composed of specific separation substances, and the separation with a specific eluent. The step of eluting the column and concentrating the eluent, etc., the above-mentioned separation column in the prior art adopts a silica gel column, because the silica gel column is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61P3/06A61P9/12C07D311/30
Inventor 李青山杨官娥朱前翔侯晋军支建民
Owner 李青山
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