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Separation purification process of monomeric compound in whitethorn leaf

A technology for separating and purifying hawthorn leaves, which is applied in the field of medicine and achieves the effects of high separation efficiency, simple and fast method, and overcoming cumbersome operations.

Inactive Publication Date: 2012-05-02
SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no application of high-speed countercurrent chromatography in the separation and purification of monomeric compounds in hawthorn leaves at home and abroad.

Method used

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  • Separation purification process of monomeric compound in whitethorn leaf
  • Separation purification process of monomeric compound in whitethorn leaf
  • Separation purification process of monomeric compound in whitethorn leaf

Examples

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Embodiment 1

[0033] 1. Prepare the crude extract of hawthorn leaves:

[0034] Take 500 g of dried hawthorn leaf crude powder, reflux extract twice with 8 times the amount of 60% ethanol for 2 hours each time, filter, combine the filtrates, concentrate under reduced pressure at 60°C until there is no alcohol smell, and obtain the crude hawthorn leaf extract.

[0035] 2. Purification:

[0036] (1) Purification with macroporous adsorption resin: take the above crude extract of hawthorn leaves, add water to suspend, and the total volume is 600ml. Add it to a 500 g pretreated 1300 macroporous adsorption resin chromatography column, and absorb for 2 hours after loading the sample. Eluted with 1500ml of water and 10% ethanol respectively (discarded). Then use 2000ml 20% ethanol to elute, after the ethanol eluted fraction is concentrated under reduced pressure, vacuum drying (60 ℃), obtains the extract powder 20.25g, and the yield is 4.1%, detects through HPLC, wherein 4 The total content of -O...

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Abstract

The invention relates to a medicine technology field, which precisely relates to the method of separating and purifying a monomer 4'' '-O-rhamnosylrutin, a vitexin-2'' -O-rhamnoside and a 4''-O-glucopyranosylvitexin from hawthorn leaves. At home or abroad, the methods of column chromatography, recrystallization etc. are generally adopted to separate and purify the effective monomers from the hawthorn leaves. The invention method comprises preparing hawthorn leaf crude extracts by immersing or refluxing the hawthorn leaves into water or ethanol water solution, using macroporous adsorption resin to wash and eliminate the water-soluble impurity respectively by water or low concentration ethanol, washing by means of the lower concentration ethanol, obtaining the hawthorn leaf macroporous adsorption resin extracts by decompressing and concentrating the eluent and separating and purifying the extracts by using the method of combining the high speed countercurrent chromatography with the preparative liquid chromatography, by which the 99 percent above purity 4'' '-O-rhamnosylrutin, vitexin-2''-O-rhamnoside and 4''-O-glucopyranosylvitexin are prepared. The preparation method of separatingand purifying a monomer 4'' '-O-rhamnosylrutin, a vitexin-2'' -O-rhamnoside and a 4''-O-glucopyranosylvitexin from hawthorn leaves is simple in operate, high in separating efficiency and excellent inproduct purity, which is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a high-purity monomer compound 4 isolated and purified from hawthorn leaves - O-rhamnosyl rutin, vitexin-2"-O-rhamnoside and 4"-O-glucose vitexin method. Background technique [0002] Hawthorn is a plant of the genus Crataegus (Crataegus.L) in the family Rosaceae. It is distributed in the northern temperate zone and is planted in Northeast my country, North China, Guangdong, Guangxi, Fujian and other places. Its leaves were first recorded as medicine in the Eastern Jin Dynasty. Pharmacological and clinical experiments have shown that flavonoids in hawthorn leaves have the effects of lowering blood pressure, lowering blood fat, increasing coronary flow, and improving blood rheology on the cardiovascular system, and have good effects on cardiovascular diseases such as myocardial ischemia and arrhythmia. curative effect. 4 of them -O-rhamnose rutin (4 -O-rhamnosylrutin), vit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/07C07H1/08A61K36/734
Inventor 范国荣周婷婷闻俊许红蕾吴玉田
Owner SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY