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Method for extracting betulic acid from cornus officinalis stones

A technology of dogwood kernels and betulinic acid is applied in the directions of steroids, organic chemistry, etc., can solve problems such as being unsuitable for large-scale production, long preparation period, small preparation scale, etc., and achieves easy operation, shortened production period, Process-less effect

Inactive Publication Date: 2012-07-11
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0005] Cornus officinalis contains betulinic acid, although it has been reported to separate betulinic acid from cornel’s fruit, because the method uses silica gel column chromatography, the operation is complicated, the preparation cycle is long, and the preparation scale is small, so it is not suitable. industrial mass production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 2.5kg of dry dogwood fruit cores, crush them properly, put them in a percolation tank, first use 25L petroleum ether for percolation extraction for 5 hours, then use 25L acetone for percolation extraction for 5 hours, collect the acetone seepage, and recover the solvent Rotary steaming to obtain 0.3kg of paste-like total extract;

[0026] Take 0.3kg of the total fruit core extract of Cornus officinalis and disperse it with 1.25L of 60% ethanol solution, and load it on the DIAIN HP-20 macroporous adsorption resin column. The resin dosage is 7.5L (volume in water), and the diameter-to-height ratio is 1:6 , adsorption flow rate 2BV / h; first use 25L 60% ethanol solution for elution, flow rate 2BV / h, then use 20L 90% ethanol solution for elution, flow rate 2BV / h, collect 90% ethanol eluate , reclaim solvent, dry, obtain the crude extract 0.045kg of betulinic acid;

[0027] Take 0.045kg of the crude extract of betulinic acid and recrystallize it in methanol to obtain 0....

Embodiment 2

[0029] Take 2.5kg of dry dogwood fruit cores, crush them properly, put them in a percolation tank, first use 15L of petroleum ether for percolation extraction for 5 hours, then use 20L of 50% acetone for percolation extraction for 8 hours, and collect 50% acetone percolation Leakage, reclaim solvent, get total extract 0.55kg;

[0030] Take 0.55kg of the total fruit pit extract of Cornus officinalis and disperse it with 1.75L of 50% ethanol solution, and load the sample on the AB-8 macroporous adsorption resin column. Flow rate 4BV / h; first use 12.5L 50% ethanol solution for elution, flow rate 4 BV / h, then use 25L 95% ethanol solution for elution, flow rate 4 BV / h, collect 95% ethanol eluate , reclaim the solvent, and dry to obtain 0.035kg of the crude extract of betulinic acid;

[0031] Take 0.035kg of the crude extract of betulinic acid and recrystallize it in methanol to obtain 0.012kg of betulinic acid with a purity of 98.1%.

Embodiment 3

[0033] Take 2.5kg of dry dogwood fruit cores, crush them properly, put them in a percolation tank, first use 25L of petroleum ether for percolation extraction for 8 hours, then use 12.5L of 70% acetone for 6.5 hours of percolation extraction, and collect 70% Acetone seepage liquid, recovery solvent drying, obtains total extract 0.45kg;

[0034] Take 0.45kg of the total fruit pit extract of Cornus officinalis and disperse it with 0.75L of 80% ethanol solution, load the sample on the AB-8 macroporous adsorption resin column, the resin dosage is 10L (volume in water), the diameter-height ratio is 1:8, 2BV / h; first eluted with 20L 80% ethanol solution at a flow rate of 3 BV / h, then eluted with 20L absolute ethanol at a flow rate of 3BV / h, collected the eluent from absolute ethanol, recovered the solvent, and dried. Get the crude extract 0.03kg of betulinic acid;

[0035] Take 0.03kg of the crude extract of betulinic acid and recrystallize it in methanol to obtain 0.01kg of betuli...

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Abstract

The invention relates to a method for extracting betulic acid from cornus officinalis stones. The method comprises the steps: firstly, the cornus officinalis stones are crushed, the crushed stones are degreased by using petroleum ether, then paste extracts are extracted by using organic solvent, the paste extracts are added to a weak-polarity or non-polar adsorption column made from macroporous adsorbent resin, high-concentration ethanol is used for elution and crude extracts of betulic acid are obtained, methanol or ethanol is used for recrystallization, and finally high-purity betulic acid is obtained. By adopting the method, betulic acid is extracted from cornus officinalis stones, not only is the extract source of betulic acid widened, but also the utilization problem of the cornus officinalis stones is loved; and simultaneously, compared with the prior art, the method has the advantages that the process is less, the production cycle is shortened by 10-30 percent, the extract purity can be up to 99 percent, and the operation is simple, thereby being favorable for mass production.

Description

technical field [0001] The invention relates to a method for extracting betulinic acid, in particular to a method for extracting betulinic acid from dogwood fruit stones. Background technique [0002] Betulinic acid is a triterpenoid compound that has anti-tumor cell growth and broad-spectrum cytotoxicity to tumor cells, such as neuroblastoma, glioma, malignant brain tumor, ovarian cancer, and lung cancer Malignant tumors and tumor cells that have developed resistance to doxorubicin have shown good activity, but no damage to normal cells. At the same time, it was found that betulinic acid has the effect on human oral epithelial cancer cells (KB), colon adenocarcinoma cells (LS-1747), liver cancer cells (SMMC-7721), lung cancer cells (A 549), HepG2, S180 sarcoma cells and human breast cancer cells. The proliferation of cells (MCF-7) can be inhibited. And there are many new mechanisms of action in anti-AIDS, which have attracted widespread attention, which makes betulinic ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
Inventor 李军姜华路西明张倩李晓明李晓宁
Owner HENAN UNIV OF SCI & TECH
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