Method for separating derivative of vitexin

A technology of vitexin and its derivatives, which is applied in the field of separation of vitexin derivatives, which can solve the problems of high cost, long cycle, and low yield, and achieve the effects of low toxicity, strong practicability, and high yield

Inactive Publication Date: 2007-10-10
LIAONING UNIV OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Literature reports are characterized by high cost, long period and low yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The mountain red leaves are crushed into coarse powder, reflux extracted with 10 times the amount of 70% ethanol for 3 times, each time for 2, 1, and 1 hour respectively, filtered, the filtrates are combined, and concentrated under reduced pressure until there is no alcohol smell. The obtained extract is removed by AB-8 macroporous adsorption resin until the sugar is no longer detected, and then eluted with 50% ethanol until the flavonoids are no longer detected. After depigmentation, n-butanol was extracted until the eluent was colorless, and n-butanol was recovered under reduced pressure until dryness. The obtained dried product was separated by silica gel column chromatography (where the silica gel was 200-260 mesh), and eluted with chloroform-methanol. All fractions (1-2 column volumes) of chloroform and methanol (4-3:1) were concentrated under reduced pressure, and the dried product was subjected to thin-layer chromatography on a silica gel column, and ethyl acetate...

Embodiment 2

[0016] Hawthorn leaves were crushed into coarse powder, refluxed with 10 times the amount of 50% ethanol and extracted twice for 2 hours each time, filtered, combined filtrates, concentrated under reduced pressure until alcohol-free. The obtained extract was removed by D101 macroporous adsorption resin until the sugar was no longer detected, and then eluted with 60% ethanol until the flavonoids were no longer detected, the alcohol eluate was concentrated under reduced pressure to no alcohol smell, and depigmented with petroleum ether Afterwards, extract n-butanol until the eluent is colorless, recover n-butanol under reduced pressure, and dry it. The resulting dried product is separated by silica gel column chromatography (where the silica gel is 200-260 mesh), eluted with chloroform-methanol, and chloroform , methanol (4-3:1) all fractions (1-2 column volumes) eluate concentrated under reduced pressure, dry matter through thin layer chromatography silica gel column, with ethyl...

Embodiment 3

[0018] The mountain red leaves are crushed into coarse powder, refluxed with 16 times the amount of 60% ethanol and extracted twice for 2 hours each time, filtered, combined filtrates, and concentrated under reduced pressure until alcohol-free. The obtained extract is removed by AB-8 macroporous adsorption resin until the sugar is no longer detected, and then eluted with 70% ethanol until the flavonoids are no longer detected. The alcohol eluate is concentrated under reduced pressure until it has no alcohol smell. After depigmentation, n-butanol was extracted until the eluent was colorless, n-butanol was recovered under reduced pressure, and dried. The dried product was separated by silica gel column chromatography (where the silica gel was 200-260 mesh), and eluted with chloroform-methanol. All fractions (1-2 column volumes) of chloroform and methanol (4-3:1) were concentrated under reduced pressure, and the dried product was subjected to thin-layer chromatography on a silica ...

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Abstract

This invention discloses a method for separating vitexin derivatives, vitexin-4'-O-glucoside and vitexin-2''-O-glucoside. The method comprises: (1) pulverizing hawthorn leaves into coarse powder, extracting by refluxing in alcohol aqueous solution, filtering, incorporating the filtrates, vacuum-concentrating to no alcohol odor, removing impurities with macroporous adsorption resin AB-8 or D101, eluting with 30-80% ethanol, vacuum-concentrating to no alcohol odor, decolorizing with petroleum ether, extracting with n-butanol, vacuum-recovering n-butanol, separating the extract by silica gel column chromatography, eluting with chloroform-methanol at a ratio of (4-3):1, vacuum-concentrating the eluate, separating by silica gel column chromatography,, eluting with ethyl acetate-butanone-methanoic acid-water or ethyl acetate-acetone-methanoic acid-water, and standing at 0-15 deg.C to obtain vitexin-4'-O-glucoside and vitexin-2''-O-glucoside. The method has such advantages as high yield, high purity, simple process and low toxicity, and is environmentally friendly.

Description

technical field [0001] The present invention relates to a method for separating vitexin derivatives: vitexin-4′-O-glucoside and vitexin-2″-O-rhamnoside by ordinary silica gel column chromatography, and the present invention particularly relates to It adopts silica gel column chromatography (the stuffing used is thin-layer chromatography silica gel), using ethyl acetate-butanone (or acetone)-formic acid-water as the eluent, and directly separates the peony from the extracts of red leaves or hawthorn leaves. Methods of Vitexin-4'-O-glucoside and Vitexin-2"-O-rhamnoside. Background technique [0002] Hawthorn leaves are the dried leaves of Crataegus pinnatifida Bge.var major N.E.Br. and C. pinnatifida Bge. of Rosaceae plants. Have blood circulation promoting and blood stasis dispelling, regulating the flow of vital energy and promoting circulation of the blood, be used for stagnation of QI and blood stasis, uncomfortable in chest, suffocation, palpitation, dizziness and tinnit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08A61K36/734A61K127/00
Inventor 英锡相张文洁郭继红
Owner LIAONING UNIV OF TRADITIONAL CHINESE MEDICINE
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