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Method for separating and purifying fraxetin and aesculetin in cortex fraxini through high-speed counter-current chromatography

A high-speed countercurrent chromatography, separation and purification technology, applied in the field of separation and purification of effective components of traditional Chinese medicine, can solve the problems of low recovery rate, sample adsorption loss, complicated operation, etc., and achieve the effects of large preparation amount, good stability and simple operation.

Pending Publication Date: 2021-07-13
SHANGHAI TAUTO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a method for separating and purifying fencetin and fencetine B in terpene by high-speed countercurrent chromatography. This method overcomes the shortcomings of traditional preparation methods such as complex operation, sample adsorption loss, and low recovery rate.

Method used

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  • Method for separating and purifying fraxetin and aesculetin in cortex fraxini through high-speed counter-current chromatography
  • Method for separating and purifying fraxetin and aesculetin in cortex fraxini through high-speed counter-current chromatography
  • Method for separating and purifying fraxetin and aesculetin in cortex fraxini through high-speed counter-current chromatography

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Experimental program
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Effect test

Embodiment 1

[0025] (1) Take Qinpi medicinal material, crush it to 40-60 mesh, extract by ultrasonic heating with 90wt% ethanol solution, heating temperature is 60°C, solid-liquid ratio is 1:6, extract twice for 60min, and rotary steam under reduced pressure to obtain Qinpi Crude extract: Disperse the crude extract of Quercus chinensis with water, extract with petroleum ether, ethyl acetate, n-butanol, filter the ethyl acetate extract, concentrate under reduced pressure to obtain the crude extract of ethyl acetate, the ethyl acetate extraction part HPLC analysis chart, such as figure 1 shown.

[0026] (2) Apply high-speed countercurrent chromatography to carry out the separation and purification of coumarin compounds to the ethyl acetate part of the obtained fenugreek:

[0027] Adopt ethyl acetate: ethanol: water=10:1:10 as solvent system, upper phase is stationary phase, lower phase is mobile phase, high-speed countercurrent chromatograph column volume is 300mL, loading sample amount 0....

Embodiment 2

[0031] (1) Take Qinpi medicinal material, crush it to 50-80 mesh, extract by ultrasonic heating with 95wt% ethanol solution, heating temperature is 70°C, solid-liquid ratio is 1:5, extract twice for 60min, and spin steam under reduced pressure to obtain Qinpi Crude extract: Disperse the crude extract of Quercus chinensis with water, extract with petroleum ether, ethyl acetate, n-butanol, filter the ethyl acetate extract, concentrate under reduced pressure to obtain the crude extract of ethyl acetate, the ethyl acetate extraction part HPLC analysis chart, such as figure 1 shown.

[0032] (2) apply high-speed countercurrent chromatography to carry out the separation and purification of coumarin compounds to the ethyl acetate part of the obtained fenugreek:

[0033]Adopt ethyl acetate: ethanol: water=10:1:8 as solvent system, upper phase is stationary phase, and lower phase is mobile phase, and high-speed countercurrent chromatograph column volume is 300mL, loading sample amoun...

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Abstract

The invention relates to a method for separating and purifying fraxetin and aesculetin in cortex fraxini through high-speed counter-current chromatography. The method comprises the following steps: (1) crushing the cortex fraxini medicinal material, heating and extracting by adopting an ethanol solution, merging filtrate, and carrying out reduced-pressure rotary evaporation to obtain a crude cortex fraxini extract; (2) dissolving the cortex fraxini crude extract obtained in the step (1), extracting with petroleum ether, ethyl acetate and n-butyl alcohol respectively, filtering extract liquor, and concentrating under reduced pressure to obtain petroleum ether, ethyl acetate, n-butyl alcohol and a water extraction section respectively; and (3) separating and purifying the ethyl acetate extraction section by adopting high-speed counter-current chromatography to obtain the fraxetin and the aesculetin. The method overcomes the defects of complex operation, sample adsorption loss, low recovery rate and the like of the traditional preparation method; and the method is high in efficiency, easy to operate, large in preparation amount and low in comprehensive cost, and has good application and popularization value.

Description

technical field [0001] The invention belongs to the field of separation and purification of effective components of traditional Chinese medicines, and in particular relates to a method for separating and purifying fencetin and fencetrin in tertiflorium bark by high-speed countercurrent chromatography. Background technique [0002] Qinpi is the dry bark or dry bark of Fraxinus rhynchophylla Hance, Fraxinuschinensis Roxb., Fraxinus szaboana Lingelsh. or Fraxinusstylosa Lingelsh. of Oleaceae plant Fraxinus rhynchophylla Hance. Clearing away heat and dampness, clearing liver and improving eyesight, relieving asthma and relieving cough. It is used for heat-toxin diarrhea, conjunctival congestion, swelling and pain, and nebula. The main active ingredients in tertiflorium are coumarins, which mainly include terperetin, terperetin, terperetin A and terperetin B. [0003] There are existing literature reports on the method of extracting, separating and preparing coumarin components...

Claims

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Application Information

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IPC IPC(8): C07D311/16
CPCC07D311/16
Inventor 王维娜邓力
Owner SHANGHAI TAUTO BIOTECH CO LTD
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