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Method for extracting isoflavonoids compound in all-grass of Twining Rhynchosia with ionic liquid

A technology of ionic liquids and isoflavones, applied in the direction of organic chemistry, etc., to achieve the effect of improving selectivity, simple method, and reducing pollution

Inactive Publication Date: 2011-03-02
HENAN UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The object of the present invention is to provide a kind of method that utilizes ionic liquid to extract the isoflavones compound in the root of Herba Versaceae, this method is simple, fast, solves the problem of using traditional phytochemical The problem that the means cannot extract and isolate the effective components in the root of Luhuo

Method used

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  • Method for extracting isoflavonoids compound in all-grass of Twining Rhynchosia with ionic liquid
  • Method for extracting isoflavonoids compound in all-grass of Twining Rhynchosia with ionic liquid
  • Method for extracting isoflavonoids compound in all-grass of Twining Rhynchosia with ionic liquid

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Experimental program
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Embodiment 1

[0021] Take 2.4g of the pulverized Rhizoma deerhusii, extract with 70% ethanol as a solvent, and obtain an extract after extraction; then mix the extract with 7% water by weight of the extract to obtain a slurry, stir at room temperature, add 1-butyl-3-methylimidazolium tetrafluoroborate with 1 times the volume of the slurry, reacted for 6 hours to obtain a solid-liquid mixture a, after the solid-liquid mixture a was centrifuged, the supernatant was taken, and the water was removed by distillation under reduced pressure 1.6 g of column chromatography sample was obtained, separated by silica gel column chromatography, gradient elution was carried out with cyclohexane / ethyl acetate and ethyl acetate / methanol as eluent, and the volume ratio was 9:1→to 0:10 respectively and 10:0 → to 6:4. The eluate was collected, tracked and monitored by thin layer chromatography (TLC), and the same fractions were combined to obtain compound 1 and compound 2, which were detected as pure spots by ...

Embodiment 2

[0025] Take 2.8g of pulverized Rhizoma deerhusii, extract it with 70% ethanol to get the extract; then mix the extract with 12% water of the weight of the extract to get a slurry, and add 1 -Butyl-3-methylimidazolium tetrafluoroborate, reacted for 10 hours to obtain a solid-liquid mixture a, after the solid-liquid mixture a was centrifuged, the supernatant was distilled under reduced pressure to remove water, and then a column chromatography sample 1.73 g, separated by silica gel column chromatography, using cyclohexane / ethyl acetate, ethyl acetate / methanol as eluents for gradient elution, the volume ratios are 9:1 → to 0:10 and 10:0 → to 6:4. The eluate was collected, tracked and monitored by TLC, and the same fractions were combined to obtain compound 1 and compound 2, which were detected as pure spots by TLC.

[0026] Structural identification of isoflavones:

[0027] Compound 1, yellow amorphous powder, 13mg. H NMR spectrum see figure 1 ( 1 H-NMR, MeOD, 400MH Z )....

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Abstract

The invention relates to a method for extracting isoflavonoids compound in all-grass of Twining Rhynchosia with ionic liquid, comprising: obtaining extractum after smashed all-grass of Twining Rhynchosia is extracted with alcohol the concentration of which is 70%; mixing the extractum with water which accounts for 7-12 wt% of extractum to obtain slurry; while stirring at room temperature, adding ionic liquid the volume of which is 1-2 times of slurry; after reacting for 6-10h, obtaining solid-liquid mixture a; and after filtrate obtained by separating the solid-liquid mixture a is dewatered, carrying out chromatographic separation by a silicagel column or a polyamide column, and obtaining isoflavonoids compound. The method of the invention is simple and quick, and utilizes [Bmim] BF4 as extraction and separation solvent to successfully separate and obtain 4'-(1''-methoxy group)-propyl group oxo-5,7-dihydroxyisoflavone and biochanin A from the all-grass of Twining Rhynchosia at room temperature, thus solving the difficulty that the traditional plant chemical means can not effectively separate and purify isoflavonoids compound in all-grass of Twining Rhynchosia.

Description

technical field [0001] The invention belongs to the field of extracting active ingredients of plants, and in particular relates to a method for extracting isoflavone compounds in deerhuscari root by using ionic liquid. Background technique [0002] Many traditional Chinese medicines have various curative effects because they contain a variety of biologically active compounds, and have been used in medicine and diet for thousands of years. Common active ingredients such as: polyphenolic compounds, nitrogenous compounds, vitamins, terpenoids and some other endogenous metabolites. These active compounds can be extracted by volatile organic solvents, thus establishing the solvent extraction and separation technology in phytochemical research. However, the organic solvents used in traditional Chinese medicine extraction methods are generally low-boiling, toxic, flammable, explosive, and volatile compounds, which not only endanger the health of operators, but also seriously pollu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/36C07D311/40
Inventor 尹卫平王键吉任运来刘普李欣任云利闫孟杰胡亚
Owner HENAN UNIV OF SCI & TECH
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