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Preparation method of high-purity prunetin

A high-purity prunin technology, applied in the field of natural medicinal chemistry, can solve the problems of cumbersome operation and poor reproducibility, and achieve the effects of simple operation, short production cycle and large preparation volume

Inactive Publication Date: 2011-11-23
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing process for preparing puracetin produces a large amount of silica gel waste during the production process, which is cumbersome to operate and poor in reproducibility

Method used

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  • Preparation method of high-purity prunetin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take Chamdo pheasant and crush it, take 10kg, put it into an ultrasonic extraction tank, add 8 times the amount of 90% ethanol for ultrasonic extraction for 40 minutes, filter the liquid, add 6 times the amount of 80% ethanol solution for ultrasonic extraction for 30 minutes, combine the extracts twice and concentrate under reduced pressure No alcohol, add appropriate amount of water to disperse, add polyamide resin column for saturated adsorption, wash the resin column with water to remove sugar color, take 7BV30% ethanol solution to elute and discard the eluent, then use 4BV80% ethanol solution to elute the target component, elute The solution was concentrated under reduced pressure and extracted three times with an equal volume of ethyl acetate, and the extract was concentrated under reduced pressure to obtain 50 ml of a concentrated solution.

[0019] Take chloroform, methanol, and phosphoric acid water (pH2) solution, mix them thoroughly in a separatory funnel accor...

Embodiment 2

[0021] Take Caragana pheasanta, take 10kg, put it into an ultrasonic extraction tank, add 6 times the amount of 80% methanol for ultrasonic extraction for 30 minutes, extract 3 times, extract the extract under reduced pressure and concentrate without alcohol, add appropriate amount of water to disperse, add polyamide resin column for saturated adsorption , after washing the resin column with water without sugar color, take 5BV50% ethanol solution to elute and discard the eluent, then use 5BV70% ethanol solution to elute the target component, and then extract the eluent with an equal volume of ethyl acetate for 4 times after concentrating under reduced pressure. The solution was concentrated under reduced pressure to obtain 60 ml of concentrated solution.

[0022] Take chloroform, methanol, and phosphoric acid water (pH3) solution, mix them thoroughly in a separatory funnel according to the ratio of 8:6:3, after standing for stratification, take the upper phase as the stationary...

Embodiment 3

[0024] Take Chamdo Caragana and crush it, take 10kg, put it into an ultrasonic extraction tank, add 5 times the amount of 70% methanol for ultrasonic extraction for 30 minutes, and extract 3 times. , after washing the resin column with water without sugar color, take 5BV50% ethanol solution to elute and discard the eluent, then use 5BV75% ethanol solution to elute the target component, and the eluate is concentrated under reduced pressure and extracted 3 times with an equal volume of ethyl acetate to extract The solution was concentrated under reduced pressure to obtain 65 ml of concentrated solution.

[0025] Take chloroform, methanol, and phosphoric acid water (pH3) solution, and mix them thoroughly in a separatory funnel according to the ratio of 8:5:3. After standing for stratification, take the upper phase as the stationary phase, fill the column of the countercurrent chromatography, and turn on the main engine. The rotating speed is adjusted to 1000rpm, and the lower pha...

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Abstract

The invention relates to a preparation method of high-purity prunetin, belonging to the field of natural pharmaceutical chemistry. The preparation method of the high-purity prunetin comprises the following steps of: (1) grinding Qamdo caragana as a raw material, ultrasonically extracting by using 5-8 times of low-carbon alcohol, concentrating an extracting solution at a reduced pressure, adding a right amount of water to the concentrated solution for dispersion, adding polyamide resin for adsorption, carrying out gradient elution by using the water and the alcohol, collecting target components, concentrating at a reduced pressure, then extracting by using ethyl acetate, and concentrating the extracting solution at a reduced pressure to obtain the concentrated solution; (2) sufficiently mixing chloroform, methanol and an acidic aqueous solution in a separating funnel, standing for layering, then taking top phases as immobile phases, filling into reflux chromatography columns, starting a principal machine, pumping bottom phases as mobile phases, injecting the concentrated solution through a sampling valve after balancing, collecting components according to a detector map, recovering regents, and drying to obtain the high-purity prunetin. The invention has the advantages of easiness in operation of a process, short production period, high yield and suitability for industrialized preparation.

Description

Technical field: [0001] The invention belongs to the field of natural medicinal chemistry, and in particular relates to a preparation method of high-purity prunus. Background technique: [0002] Prunetin is 5,4′-dihydroxy-7-methoxyisoflavone, CAS No. 552-59-0, melting point 236-238°C (methanol), molecular formula C 16 h 12 o 5 , molecular weight 284.26, molecular structure formula: [0003] [0004] Prunus is an isoflavone substance belonging to Prunus, which has anti-inflammatory and hypolipidemic effects, and also has phytoestrogens-like effects. For example, the patent "a pharmaceutical composition containing prunin and its application in medicine" and the patent "a pharmaceutical composition containing red cloverin and prunin and its application in medicine" have been experimentally confirmed. its pharmacological effects. The process of extracting prunus from plants is rarely disclosed, and most of them are research-based processes or low-content extracts. For e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/40
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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