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Separation purification process of monomeric compound in whitethorn leaf

A technology for separation and purification of hawthorn leaves, applied in the field of medicine, to achieve the effect of good product purity, overcome cumbersome operations, and be suitable for industrial production

Inactive Publication Date: 2008-07-16
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

Experimental program
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Effect test

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-mentioned crude extract of hawthorn leaves, add water and 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 eluted with 2000ml 20% ethanol, concentrated the ethanol eluted fraction under reduced pressure, and dried in vacuo (60°C) to obtain 20.25g of extract powder, with a yield of 4.1%, which was detected by HPLC, in which 4-O-mouse Th...

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PUM

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Abstract

The invention relates to 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 and so on 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 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 is simple to operate, of high separating efficiency and excellent product purity, which is suitable for industrial production.

Description

technical field [0001] The present invention relates to the technical field of medicine, in particular to a high-purity monomer compound 4-O-rhamnosin rutin, vitexin-2″-O-rhamnoside and 4″-rhamnoside isolated and purified from hawthorn leaves. 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. Among them, 4-O-rhamnosylrutin (4-O-rh...

Claims

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Application Information

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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
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