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Method for preparing high-purity quercus acutissima A

A high-purity technology of quercetin, which is applied in the field of preparation of plant active ingredients, can solve the problems of less research on quercetin A and no preparation method of quercetin A, so as to avoid chemical and structural changes and reduce polysaccharides Dissolution and good separation effect

Inactive Publication Date: 2012-09-12
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, domestic research on Quercetin A is less, and it is still in its infancy, and there is no preparation method for Quercetin A.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Crush the fresh bark of Quercus burvata, take 1kg, put it into a supercritical extraction device, extract at a temperature of 35°C and a pressure of 20MPa for 100min, add 8L of 80% ethanol solution to the residue for ultrasonic extraction, the ultrasonic frequency is 25KHz, extract 3 1 hour each time, filter, combine the extracts, concentrate, add a 3% gelatin solution, stir until no precipitation occurs, centrifuge, dissolve the precipitate with 50% acetone aqueous solution, filter out the gelatin, and obtain a preliminary purified solution. 1LHPD-400 macroporous resin column, after the adsorption is completed, first elute with 4L of water, then with 4L of 70% ethanol solution, control the flow rate at 3ml / min, collect the eluate rich in Quercetin A, concentrate, concentrate The solution was dispersed with water, put on Toyopearl HW-40 column, eluted with 65% acetone solution, acetone was recovered from the eluent, concentrated, left to stand for crystallization, and re...

Embodiment 2

[0021] Crush the fresh bark of Quercus burvata, take 1kg, put it into a supercritical extraction device, extract at a temperature of 45°C and a pressure of 30MPa for 50min, add 5L of 70% ethanol solution to the residue for ultrasonic extraction, the ultrasonic frequency is 35KHz, extract 2 1 hour each time, filter, combine the extracts, concentrate, add a 6% gelatin solution, stir until no precipitation occurs, centrifuge, dissolve the precipitate with 90% acetone aqueous solution, filter out the gelatin, and obtain a preliminary purified solution. 1LHPD-400 macroporous resin column, after the adsorption is completed, first elute with 5L of water, then elute with 5L of 70% ethanol solution, control the flow rate to 4.5ml / min, collect the eluate rich in Quercetin A, concentrate, The concentrated solution was dispersed with water, put on a Toyopearl HW-40 column, and eluted with 60% acetone solution. The acetone was recovered from the eluent, concentrated, left to stand for cryst...

Embodiment 3

[0023] Crush the fresh bark of Quercus burvata, take 1kg, put it into a supercritical extraction device, extract at a temperature of 40°C and a pressure of 30MPa for 60min, add 10L of 70% ethanol solution to the residue for ultrasonic extraction, the ultrasonic frequency is 40KHz, and extract 2 time, 2 hours each time, filter, combine the extracts, concentrate, add a 5% gelatin solution, stir until no precipitation occurs, centrifuge, dissolve the precipitate with 70% acetone aqueous solution, filter out the gelatin, and obtain a preliminary purified solution. 1LADS-17 macroporous resin column, after the adsorption is completed, first elute with 3L of water, then eluted with 6L of 70% ethanol solution, control the flow rate to 3.5ml / min, collect the eluate rich in Quercetin A, concentrate, The concentrate was dispersed with water, put on the MCl-gel CHP-20P column, and eluted with 80% acetone solution. The acetone was recovered from the eluent, concentrated, left to stand for c...

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PUM

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Abstract

The invention discloses a method for preparing high-purity quercus acutissima A. Fresh barks of quercus acutissima are adopted to serve as a raw material in the method. The method comprises (1) utilizing supercritical carbon dioxide fluid to extract oil materials in the fresh barks of quercus acutissima, and obtaining extraction liquid after ultrasonic extraction; (2) concentrating the extraction liquid, adding gelatin solution, carrying out centrifugation, utilizing acetone aqueous solution to dissolve sediments, removing gelatin by extraction, and obtaining primary purification liquid; (3) purify the primary purification liquid through macroporous resin, utilizing water and ethanol water to perform elution, and concentrating eluent; and (4) separating concentrated solution through gel column chromatography, utilizing acetone solution of 60%-80% to perform elution, collecting eluent, carrying out decompression concentration and standing crystallization, and obtaining the quercus acutissima A by recrystallization. The method lays a foundation for intensive study of pharmacological activity and pharmaceutical preparation of the quercus acutissima A.

Description

technical field [0001] The invention relates to a method for preparing plant active ingredients, in particular to a method for preparing quercetin A from the fresh bark of Quercus quercus. Background technique [0002] Quercetin A is a tannin substance with the molecular formula C 56 h 38 o 31 , with a molecular weight of 1206.89, exists in the Fagaceae Quercus Quercus acutissima In the fresh bark of Carruth. [0003] Modern studies have shown that quercetin A has cytotoxic activity on melanoma (RPMI-7951), and its ED 50 0.61μg / ml; inhibitory activity on topoisomerase Ⅱ, IC 50 0.2 μM. [0004] At present, the domestic research on quercetin A is less, and it is still in its infancy, and there is no preparation method of quercetin A. Therefore, it is very necessary to develop a method for preparing high-purity Quercerin A, which is of great significance for expanding drug sources and comprehensive utilization of Quercus Quercus. Contents of the invention [0005] Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/22
CPCY02P20/54
Inventor 刘东锋万冬梅
Owner NANJING ZELANG MEDICAL TECH
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