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A method for separating and purifying lupeol from pear wood

A technology for separation and purification of lupeol, applied in organic chemistry, steroids, etc., can solve the problems of low yield, unfavorable industrial production, and long production cycle of column chromatography, so as to reduce production cost and avoid inclusion phenomenon , to achieve the effect of comprehensive utilization

Active Publication Date: 2021-03-12
SHAANXI JIAHE PHYTOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for separating and purifying lupeol from pear wood, so as to solve the problems that the prior art uses column chromatography with long production cycle and low yield, which is unfavorable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A method for separating and purifying lupeol from pear wood, comprising the following steps:

[0028] 1) Enzymatic hydrolysis:

[0029] Take 100kg of sand pear wood raw material and crush it, soak it in 300kg of water, add 50g of cellulase to enzymolyze it at 40°C for 90min, and filter to obtain the enzymolysis material.

[0030] 2) Extract:

[0031] The above enzymolysis material was extracted with 800kg of 80% ethanol under reflux, the extract was concentrated under reduced pressure to an alcohol content of 30%, 20kg of 767 activated carbon and 10kg of activated clay were added for adsorption at 60°C for 1 hour, filtered, and the insoluble matter was collected.

[0032] 3) Crystallization and drying:

[0033] Heat the above insoluble matter with 96kg of dichloromethane, filter, and absorb the filtrate with a prepared sodium chloride column, concentrate the adsorption effluent to 1.9kg, add isopropanol until the solution is slightly turbid, and keep warm at 10-15°C f...

Embodiment 2

[0037] A method for separating and purifying lupeol from pear wood, comprising the following steps:

[0038] 1) Enzymatic hydrolysis:

[0039] Take 100 kg of sand pear wood raw material and crush it, soak it in 500 kg of water, add 100 g of hemicellulase to enzymolyze it at 50°C for 60 minutes, and filter to obtain the enzymolysis material.

[0040] 2) Extract:

[0041] The above enzymolysis material was extracted with 1500kg of 70% methanol under reflux, the extract was concentrated under reduced pressure to an alcohol content of 40%, 30kg of 320 activated carbon and 15kg of activated clay were added for adsorption at 80°C for 3 hours, filtered, and the insoluble matter was collected.

[0042] 3) Crystallization and drying:

[0043] Thermally dissolve the above insoluble matter with 227kg of ethyl acetate, filter, and absorb the filtrate with a pre-prepared sodium chloride column, concentrate the adsorption effluent to 5.6kg, add amyl alcohol until the solution is slightly ...

Embodiment 3

[0047] A method for separating and purifying lupeol from pear wood, comprising the following steps:

[0048] 1) Enzymatic hydrolysis:

[0049] Take 100 kg of sand pear wood raw material and crush it, soak it in 400 kg of water, add 80 g of cellulase to enzymolyze it at 45°C for 70 minutes, and filter to obtain the enzymatic hydrolyzed material.

[0050] 2) Extract:

[0051] The above enzymatic hydrolysis material was extracted with 1000kg 75% acetone under reflux, the extract was concentrated under reduced pressure to an alcohol content of 35%, 25kg 303 activated carbon and 12kg activated clay were added for adsorption at 70°C for 2 hours, filtered, and the insoluble matter was collected.

[0052] 3) Crystallization and drying:

[0053] Dissolve the above insoluble matter with 135kg of dichloromethane, filter, and absorb the filtrate with a pre-prepared anhydrous copper sulfate column, concentrate the adsorption effluent to 3kg, add n-butanol until the solution is slightly t...

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PUM

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Abstract

The invention relates to a method for separating and purifying lupeol from crataeva nurvala and belongs to a plant purification method. The method is adopted for solving the problems of long production period, low yield and being adverse to industrial production of column chromatography adopted in the prior art. According to the technical scheme, the method for separating and purifying lupeol fromcrataeva nurvala comprises the following steps: treating a crataeva nurvala raw material through enzymolysis; absorbing active ingredients by activated carbon and activated clay; dehydrating with sodium chloride; crystallizing with mixed solvent; cleaning impurities with ultralow polarity reagent, thereby acquiring a lupeol product. According to the invention, an enzyme reagent is added for enzymolysis, so that the yield of lupeol is effectively promoted; active ingredients are absorbed by activated carbon and activated clay, so that the separation of active ingredients and impurities can bequickly realized; the process route is simplified; the production cost is effectively lowered; the production efficiency is increased; the dosage of toxic reagent is reduced; green production can be realized.

Description

technical field [0001] The invention belongs to a plant purification method, in particular to a method for separating and purifying lupeol from pear wood. Background technique [0002] Sand pear wood is also called spiny fish wood. It is mainly produced in Yunnan, Guangxi, Guangdong and other provinces of China. It is distributed in the Indochina Peninsula of India to Indonesia. It has been included in Hainan Flora. It has anti-oxidation, anti-inflammation, and promotion of wound healing. effect. A study led by the University of Hong Kong found that lupeol can inhibit the growth and spread of head and neck tumors, and may also have therapeutic effects on liver, prostate and breast cancers. [0003] Document "Effect of lupeol isolated from Crataeva nurvala Buch.-Ham.stembark extract against free radical induced nephrotoxicity in rat." IndianJournal of Experimental Biology Vol.42, July, 2004, pp.686-690. The method for separating and purifying lupeol from pear wood, the raw ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00
CPCC07J63/008
Inventor 张瑜肖红郭文华王晓莹
Owner SHAANXI JIAHE PHYTOCHEM
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