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Method for preparing tetrahydroxy diphenyl ethylene glycoside separated from fleece-flower root

A technology of tetrahydroxystilbene and stilbene glycosides, which is applied in the field of phytochemistry, can solve problems such as difficult industrial production, large sample loss, and increased costs, and achieve the effects of simple operation, improved stability, and cost savings

Inactive Publication Date: 2007-07-25
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] There are defects in the above extraction methods: one may lead to the production of more non-prototype metabolites (some sensitive functional groups are oxidized and deteriorated, such as phenolic hydroxyl groups); In addition, a large amount of solvent elution will also greatly increase the cost, and it is difficult to industrialize production

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0018] Pulverize the tubers of Polygonum multiflorum, sieve through 20 mesh, weigh 500g into the reactor, add 4500ml of 60% ethanol, stir, extract for 60min, filter, collect the extract, extract the residue again under the same conditions, and combine the two extracts , concentrated under reduced pressure to remove ethanol. The concentrated solution is separated by a polyamide chromatography column, ethanol gradient elution, followed by thin-layer chromatography for detection, and the stilbene glycoside components are collected. Concentrate the collected components to a paste under reduced pressure, add the solvent acetone-water (1:5) (volume) and use the solvent crystallization method to prepare a supersaturated solution at room temperature, slowly lower the temperature, slowly evaporate the solvent to precipitate crystals, After suction filtration, the crude crystals were recrystallized under the same conditions to obtain white needle-like crystals of stilbene glycosides.

Embodiment 2

[0020] Pulverize tubers of Polygonum multiflorum, sieve through 20 meshes, weigh 500g into the reactor, add 7500ml of water, stir at 50°C, extract for 40min, filter, collect the extract, extract the residue again under the same conditions, combine the two The secondary extract was concentrated under reduced pressure, flocculated with chitosan, centrifuged, and the supernatant was concentrated under reduced pressure. The concentrated solution is separated with macroporous adsorption resin HPD100, ethanol gradient elution, followed by thin-layer chromatography for detection, and the stilbene glycoside components are collected. Concentrate the collected components to a paste under reduced pressure, add the solvent n-butanol-water (1:6) (volume), use the solvent crystallization method, prepare a supersaturated solution at room temperature, slowly lower the temperature, and slowly evaporate the solvent Crystals were precipitated, and after suction filtration, the crude crystals wer...

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PUM

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Abstract

This invention relates to a method for separating and preparing tetrahydroxy distyrene glucoside from Polygonum multiflorum. The method comprises: (1) pulverizing Polygonum multiflorum tubers, sieving to 20 mesh, extracting with water or ethanl, and concentrating the extract; (2) separating the concentrated extract with polyamide or macroporous adsorbent resin chromatographic column, eluting with ethanol, detecting by thin-layer chromatography, and collecting distyrene glucoside component; (3) vacuum-concentrating, preparing saturated solution at room temperature, cooling slowly, evaporating the solvent to precipitate crystals, vacuum-filtering, and recrystallizing to obtain white needle-like crystals of distyrene glucoside. The method has such advantages as easy operation, and high product purity.

Description

technical field [0001] The patent of the present invention relates to the field of phytochemistry, the separation and preparation process of natural active ingredients in Chinese herbal medicine. Background technique [0002] At present, the reports about stilbene glycosides in Radix Polygoni Multiflori are all white amorphous substances. As for the separation of pure stilbene glycosides, the literature reports all select different kinds of chromatographic supports and repeat column chromatography for many times to finally obtain pure stilbene glycosides. [0003] For example, in the separation of stilbene glycosides, ethanol reflux extraction is used in China, the ethanol extract is recovered, and then extracted by ether cold soaking, and the pH gradient method is used to extract emodin, emodin methyl ether and other components from the ether extract. The alcoholic extract extracted with ether is refluxed with water and ethyl acetate for several times, and then repeatedly ...

Claims

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Application Information

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IPC IPC(8): C07H15/20C07H1/08A61K36/704A61K125/00
Inventor 吕丽爽
Owner NANJING NORMAL UNIVERSITY
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