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Method for separating magnolol and honokiol from magnolia bark

A technology with honokiol and honokiol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of difficult to obtain compound monomers, pollution, tailing, etc., and achieve a large amount of separation , solvent saving, no sample loss effect

Inactive Publication Date: 2005-10-26
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, magnolol and honokiol are isomers with similar properties. When using traditional separation techniques such as thin-layer chromatography and column chromatography, tailing, pollution, and loss often occur due to the adsorption of solid carriers. , it is difficult to obtain higher purity compound monomers

Method used

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  • Method for separating magnolol and honokiol from magnolia bark
  • Method for separating magnolol and honokiol from magnolia bark
  • Method for separating magnolol and honokiol from magnolia bark

Examples

Experimental program
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Effect test

Embodiment 1

[0020] 1. Heat and reflux 5kg of dried magnolia bark powder with 10L of 65% ethanol for 3 times, each time for 2 hours, filter out the solvent, add 10L of 65% ethanol to the filter residue, repeat the above operation three times, and combine the extracts Concentrate under reduced pressure with a vacuum rotary evaporator to obtain an extract, the concentration temperature is 40 ° C, and after drying, 85 g of crude Magnolia officinalis is obtained. Its composition structure and content are as follows figure 1 As shown, the contents of honokiol and magnolol are 55.4% and 40.1%, respectively.

[0021] 2. Separate Magnolia officinalis extract with countercurrent chromatography. Use petroleum ether, ethyl acetate, carbon tetrachloride, methanol and water to prepare a two-phase solvent in a volume ratio of 1:1:8:6:1, and separate the upper and lower phases by standing in a liquid separation container. Dissolve 1500 mg of Magnolia officinalis in 7 ml of the upper phase and 7 ml of t...

Embodiment 2

[0023] The preparation method of the crude Magnolia officinalis is the same as in Example 1, and the Magnolia officinalis extract is separated by countercurrent chromatography. Prepare a two-phase solvent with ethyl acetate, carbon tetrachloride, methanol and water in a volume ratio of 1:6:4:1, and separate the upper and lower phases by standing in a liquid separation container. Dissolve 500 mg of magnolia bark in 5 ml of the upper phase and 5 ml of the lower phase to form a sample solution. The internal diameter of the countercurrent chromatographic column is 4mm, and the column volume is 1600ml. The above phase is used as the stationary phase, and the lower phase is the mobile phase. After the separation column of the countercurrent chromatograph is filled with the stationary phase, the sample solution is injected into the sampling loop of the countercurrent chromatograph, and the countercurrent chromatograph is turned on at a speed of 300 rpm. The flow velocity of 5ml / min ...

Embodiment 3

[0025] The preparation method of the crude Magnolia officinalis is the same as in Example 1, and the Magnolia officinalis extract is separated by countercurrent chromatography. Prepare a two-phase solvent with diethyl ether, ethyl acetate, carbon tetrachloride, methanol and water at a volume ratio of 0.5:0.5:5:4:1, and separate the upper and lower phases by standing in a liquid separation container. Dissolve 180 mg of crude Magnolia officinalis in 3 ml of the upper phase and 3 ml of the lower phase to form a sample solution. The internal diameter of the countercurrent chromatographic column is 2mm, and the column volume is 380ml. The above phase is used as the stationary phase, and the lower phase is the mobile phase. After the separation column of the countercurrent chromatograph is filled with the stationary phase, the sample solution is injected into the sampling loop of the countercurrent chromatograph, and the countercurrent chromatograph is turned on at a speed of 600 rp...

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Abstract

The method for separating magnolol and honokial from Chinese medicinal material magnolia bark includes the following steps: (1) using organic solvent to repeatedly extract magnolia bark powder, combining extracts, concentrating, drying to obtain magnelia bark crude product; (2) pouring thue solvent white can be used in counter-current chromatographic separation into liquid separator so as to form mutually-insoluble two phase of solvent; (3) dissolving magnolia bark crude product in equivolume two-phase mixed solvent in the step (2); and (4), injecting one phase of two phase of solvent into separation column of counter-current chromatograph as immobile phase, injecting the solution obtained in step (3) into sample-injecting ring of coutner-current chromatograph, starting the counter-current chromatograph, and injecting another phase of two phase of solvent as mobile phase, making continuous separation and collection so as to respectively obtain purified magnolol and honokiol.

Description

technical field [0001] The invention relates to a method for separating magnolol and honokiol from magnolia bark, in particular to a method for separating and preparing monomeric magnolol and honokiol from crude magnolia bark by countercurrent chromatography. Background technique [0002] Magnolol of structural formula 1 and honokiol of structural formula 2 are two main components in magnolia bark. [0003] [0004] Formula 1 Formula 2 [0005] Magnolia officinalis is the dried bark of magnolia bark, one of the important traditional Chinese medicines in my country. It has the following medicinal effects: (1) Promoting qi and reducing swelling: used for abdominal distension or abdominal fullness pain, distension and pain. (2) Warming middle-dampness and drying dampness: used for epigastric fullness, vomiting and diarrhea caused by dampness and turbidity. (3) Lowering the Ni and relieving asthma: It is used for cough and asthma caused by ascending lung Qi. A large number...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/21
Inventor 潘远江卢延斌
Owner ZHEJIANG UNIV
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