Method for extracting and separating wedelolactone from herba ecliptae

A technology of wemarolide and Eclipta chinensis is applied in the field of extraction and separation of coumarin compounds, can solve the problems of unsuitability for industrialized production, complex extraction steps, low yield and the like, and achieves easy operation, simple process and high yield. Effect

Active Publication Date: 2015-03-04
SHAANXI JIAHE PHYTOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] In the prior art, the method for extracting wedelolide from Eclipta chinensis raw material has complex extraction steps and low yield, which is not suitable for industrialized production

Method used

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  • Method for extracting and separating wedelolactone from herba ecliptae
  • Method for extracting and separating wedelolactone from herba ecliptae
  • Method for extracting and separating wedelolactone from herba ecliptae

Examples

Experimental program
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Effect test

Embodiment 1

[0040] 10 kg of Eclipta chinensis raw material is crushed, extracted with water for 1 hour, and extracted twice at a temperature of 25°C. The filtrate was discarded, and the extract residue was filtered to dryness.

[0041] The extraction residue was extracted with 5 times the mixed solvent of petroleum ether and ethyl acetate with a mass ratio of 9:1, and the extraction temperature was 20°C. During the extraction process, 0.01% of the raw material mass was added to BHT, extracted for 2 hours, and concentrated for later use.

[0042] The diameter of the pretreatment column is 10cm, and the height is 50cm. The filler used is alumina. The conventional column filler is silica gel and C18, and its mass ratio is 1:1. The elution solvent is a mixed solvent of n-hexane and ethyl acetate. The ratio is 4:1, the eluate containing the active ingredient is collected, concentrated to 1 / 100 of the eluate, and left to crystallize.

[0043] The crystalline sample was dissolved in ethyl aceta...

Embodiment 2

[0045] 10 kg of Eclipta chinensis raw material was crushed, extracted with 5% ethanol for 1.5 h, and extracted twice at a temperature of 60°C. The filtrate was discarded, and the extract residue was filtered to dryness.

[0046] The extraction residue was extracted with ethyl acetate 5 times the mass of the raw material, and the extraction temperature was 60°C. During the extraction process, sodium metabisulfite of 1% mass of the raw material was added, extracted for 4 hours, and concentrated for later use.

[0047] The diameter of the pretreatment column is 50cm, the height is 50cm, the filler used is D204, the conventional column filler is MM500, the elution solvent is petroleum ether: ethyl acetate: methanol = 4:1:3, and the eluent containing the active ingredient is collected , concentrated to 1 / 10 of the eluate, and left to crystallize.

[0048] The crystalline sample was dissolved in acetone with 6 times the crystalline mass, concentrated to 0.1 times the crystalline ma...

Embodiment 3

[0050] 100 kg of Eclipta chinensis raw material was crushed, extracted with 50% ethanol for 2 hours, and extracted twice at a temperature of 30°C. The filtrate was discarded, and the extract residue was filtered to dryness.

[0051] The extraction slag is extracted with n-butane that is 4 times the mass of the raw material, and the extraction temperature is 40°C. During the extraction process, 0.1% of the mass of the raw material is added as a mixed antioxidant. The antioxidant is a mixed antioxidant of sodium pyrosulfite and VC. The mass of the two The ratio is 1:5, extract for 3 hours, concentrate for later use.

[0052] The diameter of the pretreatment column is 20cm, and the height is 50cm. The filler used is 001×7. The conventional column filler is silica gel, and the elution solvent is ethyl acetate:ethanol=95:5. Collect the eluate containing the active ingredient and concentrate it to 1 / 50 of the eluent, set aside for crystallization.

[0053] Dissolve the crystalline...

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Abstract

The invention relates to a method for extracting and separating wedelolactone from herba ecliptae. The method comprises the following steps: primary extraction, secondary extraction, tandem column separation and crystallization and is characterized by grinding a raw material herba ecliptae, carrying out extraction, carrying out tandem column separation and then carrying out crystallization, thus obtaining required wedelolactone. The method for extracting wedelolactone from the raw material herba ecliptae is simple to operate, has the advantages of high product content and high recovery rate and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of extraction and separation of coumarin compounds, and relates to a method for extracting and separating wedelolide, in particular to a method for extracting and separating wedelide from Eclipta chinensis. Background technique [0002] Herba Eclipta e (Her ba Eclipta e) is the dry above-ground part of the genus Channa in the family Asteraceae. It is commonly known as Eclipta, and is one of the commonly used traditional Chinese medicines. It has the functions of nourishing the liver and kidney, cooling blood and stopping bleeding. In recent years, studies at home and abroad have found that Eclipta has a strong hepatoprotective effect. For example, Wagner et al. have found that its coumarin compounds have a strong effect on liver cells of rats induced by carbon tetrachloride and lactosamine through research on the chemical components of Eclipta. Toxicity has obvious hepatoprotective and regenerative effects. At presen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 肖红王晓莹张瑜张利娜郭伟妮
Owner SHAANXI JIAHE PHYTOCHEM
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