Preparation method and content measurement method of Daphne giraldii Nitsche total coumarin extract

A technology of total coumarin and extract, which is applied in the field of natural medicinal chemistry, can solve the problems of low actual content of active ingredient coumarin compounds and inaccurate detection of coumarin compound content, etc.

Active Publication Date: 2012-05-23
GUANGZHOU LIXIN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the impurity content in the extract prepared in this patent application is high and mostly flavonoids. Absorbed, resulting in inaccurate detection of the content of coumarin compounds, the actual content of active ingredients coumarin compounds is low

Method used

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  • Preparation method and content measurement method of Daphne giraldii Nitsche total coumarin extract
  • Preparation method and content measurement method of Daphne giraldii Nitsche total coumarin extract
  • Preparation method and content measurement method of Daphne giraldii Nitsche total coumarin extract

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 1.0 kg of Zumima medicinal material, extract 3 times with 20% (volume / volume) ethanol aqueous solution under reflux, filter, combine the filtrate to recover ethanol, mix into starch, reflux extract with water-saturated n-butanol, recover solvent, add water to absorb solid matter In D201 resin, wash with water to remove impurities, then elute with 20% (volume / volume) ethanol aqueous solution, collect eluate, recover ethanol in the first half, and use the solid for later use; recover ethanol in the second half, add water to suspend the solid, and wash Ester extraction, recovering the solvent from the organic layer to obtain a solid, combining the two parts of the eluate to obtain the solid substance after treatment, and drying to obtain the effective fraction of the total coumarin of Zumima.

[0025] Determination according to high performance liquid chromatography:

[0026] Accurately weigh 50 mg of the effective fraction of Zushima total coumarin extract, put it in...

Embodiment 2

[0032]Take 1.0 kg of zushima medicinal material, extract by percolation with 30% (volume / volume) ethanol aqueous solution, recover ethanol from the percolation liquid under reduced pressure, mix it into micropowder silica gel, extract by percolation with ethyl acetate, recover the solvent, and add water to absorb the solid matter In the D201 resin, wash away impurities with 10% (volume / volume) ethanol aqueous solution, then elute with 30% (volume / volume) ethanol aqueous solution, collect the eluate, recover ethanol under reduced pressure at 60°C in the first half, and save the solid matter for later use; In the second half, ethanol is recovered under reduced pressure at 60°C, the solid substance is suspended with water, extracted with n-butanol, the solvent is recovered from the organic layer to obtain a solid, and the solid substance obtained after the treatment of the two parts of the eluent is combined, dried in vacuo to obtain Zushima total coriander The effective part of t...

Embodiment 3

[0038] Take 1.0 kg of zushima medicinal material, extract with 40% (volume / volume) ethanol aqueous solution under reflux, recover ethanol from the extract under reduced pressure, mix it into diatomaceous earth, extract with n-butanol percolation, recover the solvent, and add water to absorb the solid matter in D101 resin, wash away impurities with 20% (volume / volume) ethanol aqueous solution, then elute with 40% (volume / volume) ethanol aqueous solution, collect the eluate, reclaim ethanol in the first half, and solid matter for standby; reclaim ethanol in the second half , the solid substance is suspended with water, extracted with ethyl acetate, the solvent is recovered from the organic layer to obtain a solid, the solid substance obtained after the two parts of the eluent are combined, and vacuum-dried to obtain the effective fraction of total coumarin of Zushima.

[0039] Determine according to the above-mentioned high-performance liquid chromatography:

[0040] According t...

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Abstract

The invention provides a preparation method and a content measurement method of a Daphne giraldii Nitsche total coumarin extract. The preparation method comprises: performing extraction by using a Daphne giraldii Nitsche herbal medicament as a raw material and water and / or C1 to C5 lower alcohol as a solvent to obtain an extract; mixing the extract with a solid diluent, adding an organic solvent for extraction, recovering the solvent to obtain a solid extract, or adding the extract into water for suspension, adding the organic solvent for extraction and receovering the solvent to obtain the solid extract; adding the solid extract into water for suspension, performing chromatography by macroporous adsorption resin in a way of eluting by using water or the aqueous solution of the C1 to C5 lower alcohol as a flowing phase to remove impurities first, then using the aqueous solution of the lower alcohol for elution and finally collecting eluent; reclaiming the solution from a previous halfpart of eluent to obtain a solid which is part of the Daphne giraldii Nitsche total coumarin extract; and reclaiming the solution from the later half part of eluent to obtain a solid, adding water into the solid for suspension, extracting the solid with an organic solvent and recovering an organic layer to obtain the solid which is the other part of the Daphne giraldii Nitsche total coumarin extract.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, and mainly relates to a preparation method and a content determination method of a total coumarin extract of Zushima. Background technique [0002] Zushi Ma is the root bark and stem bark of Daphne giraldii Nitsche, a plant belonging to the genus Daphne in the family Thymelaeaceae. It has the effects of dispelling wind and collaterals, removing blood stasis and relieving pain. Folks are used to treat headaches, toothaches, rheumatoid arthritis, bruises, stomach pains, liver pains, and bronchitis. Modern pharmaceutical research shows that Zushima contains a variety of chemical components, such as coumarins (daphnetin and daphnetin, etc.), diterpenoids (daphnetin, 12-hydroxy daphnein, daphnetin A, daphnetin B, daphnetin, etc.) Daphnein, etc.), lignins ((±)-syringaresinol, (-)-pineresinol, (-)-dihydrosesamin, (-)-larixisinol, etc.), flavonoids, anthracene Chemical components such as quin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K36/83A61P19/02A61P19/04A61P29/00G01N30/36G01N21/31A61K135/00A61K125/00
Inventor 马莉韩峰侯文彬高静张新鑫申秀萍王圣明胡金芳刘静
Owner GUANGZHOU LIXIN PHARM CO LTD
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