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Method for separating and preparing robinin monomer from wild chrysanthemum flowers

A technology of wild chrysanthemum and locustin, applied in the direction of organic chemistry, can solve the problems of unsatisfactory separation effect, long separation period and other problems that have not yet been reported on the technology of locustin monomer, so as to promote the phagocytosis of white blood cells, shorten the separation period and improve the reaction conditions easily controlled effects

Inactive Publication Date: 2013-07-10
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of column chromatography are: long separation period, low recovery rate, high cost, and unsatisfactory separation effect
[0006] However, in the existing methods, there are no relevant technical reports on the separation of acacinin monomers in wild chrysanthemums using high-speed countercurrent chromatography

Method used

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  • Method for separating and preparing robinin monomer from wild chrysanthemum flowers
  • Method for separating and preparing robinin monomer from wild chrysanthemum flowers
  • Method for separating and preparing robinin monomer from wild chrysanthemum flowers

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Embodiment 1

[0031] The solvent system of this embodiment, by volume, n-hexane:ethyl acetate:methanol:water is 6:4:5:5.

[0032] The method for separating and preparing acacinin from wild chrysanthemums comprises the following steps:

[0033] a, sample: take 1Kg of wild chrysanthemum that is crushed to coarse powder, add 3 times the amount of 80% ethanol to soak at room temperature for 3 times, each time for 1 week, extract the liquid through suction filtration to obtain the clear liquid, and after the clear liquid decompresses and recovers the ethanol, Pass through the macroporous resin (AB-8), ethanol gradient elution, combine the eluent containing acaciacin, and recover ethanol under reduced pressure to obtain an aqueous solution; add 2.5 times the amount of 3mol / L hydrochloric acid to the aqueous solution, and heat The hydrolyzate was further acid hydrolyzed to obtain a black solid hydrolyzate on the wall, and the hydrolyzate was ultrasonically extracted with chloroform, and the chloro...

Embodiment 2

[0040] The solvent system of this embodiment, by volume, n-hexane:ethyl acetate:methanol:water is 7:3:5:5.

[0041] The method for separating and preparing acacinin from wild chrysanthemums comprises the following steps:

[0042] a, sample: take 1Kg of wild chrysanthemum that is crushed to coarse powder, add 3 times the amount of 80% ethanol to soak at room temperature for 3 times, each time for 1 week, extract the liquid through suction filtration to obtain the clear liquid, and after the clear liquid decompresses and recovers the ethanol, Pass through the macroporous resin (AB-8), ethanol gradient elution, combine the eluent containing acaciacin, and recover ethanol under reduced pressure to obtain an aqueous solution; add 2.5 times the amount of 3mol / L hydrochloric acid to the aqueous solution, and heat The hydrolyzate was further acid hydrolyzed to obtain a black solid hydrolyzate on the wall, and the hydrolyzate was ultrasonically extracted with chloroform, and the chloro...

Embodiment 3

[0049] The solvent system of this embodiment, by volume, n-hexane: ethyl acetate: methanol: water is 1:1:1:1.

[0050] The method for separating and preparing acacinin from wild chrysanthemums comprises the following steps:

[0051] a, sample: take 1Kg of wild chrysanthemum that is crushed to coarse powder, add 3 times the amount of 80% ethanol to soak at room temperature for 3 times, each time for 1 week, extract the liquid through suction filtration to obtain the clear liquid, and after the clear liquid decompresses and recovers the ethanol, Pass through the macroporous resin (AB-8), ethanol gradient elution, combine the eluent containing acaciacin, and recover ethanol under reduced pressure to obtain an aqueous solution; add 2.5 times the amount of 3mol / L hydrochloric acid to the aqueous solution, and heat The hydrolyzate was further acid hydrolyzed to obtain a black solid hydrolyzate on the wall, and the hydrolyzate was ultrasonically extracted with chloroform, and the chl...

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Abstract

The invention provides a method for separating and preparing robinin monomer from wild chrysanthemum flowers, relates to a method for processing wild chrysanthemum flowers, and provides a high separation efficiency and high recycling rate method for separating and preparing robinin from wild chrysanthemum flowers by adopting the high-speed counter-current chromatography. The method comprises the following steps of: 1) preparing a solvent system which forms a stationary phase and a moving phase, wherein the solvent system consists of normal hexane, ethyl acetate, methanol and water; 2) filling the stationary phase by using high-speed counter-current chromatographic instrument, and adjusting the moving speed of the moving phase and the rotating speed of a host, and pumping the moving phase for balancing; 3) feeding a sample by a feed valve; and 4) collecting a target component, reducing pressure, evaporating to dryness and re-crystallizing to obtain the robinin monomer.

Description

technical field [0001] The invention relates to a processing method of wild chrysanthemum, in particular to a method for separating and preparing acacin monomer from wild chrysanthemum by high-speed countercurrent chromatography. Background technique [0002] Wild chrysanthemum is the dry flower head of Chrysanthemum indicum L. in Compositae. In my country, it is rich in Jilin, Liaoning, Hebei, Shanxi and other places. my country has a long history of research on wild chrysanthemums. It is recorded in "Chinese Pharmacopoeia" (2010 edition) that wild chrysanthemums have the effects of clearing away heat and detoxification, purging fire and calming the liver. Modern pharmacology proves that wild chrysanthemum has broad-spectrum antibacterial, antihypertensive, increased coronary blood flow, anti-virus, and scavenging oxygen free radicals (Zhang Jie, Tan Shengjian, Jiang Ren, etc., research progress of wild chrysanthemum, Chinese New Medicine, 2004, 3(1):8-10). Wild chrysant...

Claims

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Application Information

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IPC IPC(8): C07D311/30C07D311/40
Inventor 王秀敏连惠龙杨钦磊陈庆刘泽华邱彦
Owner XIAMEN UNIV
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