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Method for extracting and separating betulinic acid from water chestnut skin

A technology of water chestnut bark and betulinic acid, applied in the directions of steroids, organic chemistry, etc., can solve unseen problems and achieve the effects of low production cost, high product purity and good separation effect

Active Publication Date: 2016-05-18
广西嘉宝食品集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In our research, we found that water chestnut skin is rich in betulinic acid, but there is no literature report on the extraction and isolation of this compound from water chestnut skin

Method used

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  • Method for extracting and separating betulinic acid from water chestnut skin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) In the extraction tank, add 800g of water chestnut skin powder and 8.0L of 70% by volume methanol aqueous solution, extract at 70°C for 2 hours, filter, and extract 3 times in total, combine the filtrates, concentrate under reduced pressure into a paste, and obtain the extract 138g.

[0022] (2) Add 800 mL of water to the extract to make a turbid liquid, then add 1.6 L of ethyl acetate to extract 3 times, combine the extracts, concentrate under reduced pressure, and obtain 11.5 g of the extract.

[0023] (3) Add 30mL of methanol to the extract until completely dissolved, add 30g of silica gel to mix the sample, separate by silica gel column chromatography, elute with petroleum ether-ethyl acetate solution with a volume ratio of 8:2, detect by thin layer chromatography, and collect The eluents containing betulinic acid were combined and concentrated under reduced pressure to obtain 1.82 g of crude product.

[0024] (4) Dissolve the crude product in 10 mL of hot etha...

Embodiment 2

[0026] (1) In the extraction tank, add 800g of chestnut skin powder and 6.4L of 90% ethanol aqueous solution by volume, extract at 80°C for 2.5 hours, filter, and extract 3 times in total, combine the filtrates, concentrate the paste under reduced pressure, and obtain the extract 115g.

[0027] (2) Add 1.0 L of water to the extract to make a turbid liquid, add 2.0 L of ethyl acetate to extract 3 times, combine the extracts, concentrate under reduced pressure, and obtain 10.3 g of the extract.

[0028] (3) Add 30mL of methanol to the extract until completely dissolved, add 30g of silica gel to mix the sample, separate by silica gel column chromatography, elute with petroleum ether-ethyl acetate solution with a volume ratio of 8.5:1.5, detect by thin layer chromatography, and collect The eluents containing betulinic acid were combined and concentrated under reduced pressure to obtain 1.76 g of crude product.

[0029] (4) Dissolve the semi-finished product in 10 mL of hot ethano...

Embodiment 3

[0031] (1) In the extraction tank, add 800g of water chestnut skin powder and 6.4L of 70% by volume acetone aqueous solution, extract at 50°C for 2 hours, filter, extract 3 times in total, combine the filtrates, concentrate under reduced pressure into a paste, and obtain the extract 115g.

[0032] (2) Add 800 mL of water to the extract to make a turbid liquid, then add 1.6 L of ethyl acetate to extract 3 times, combine the extracts, concentrate under reduced pressure, and obtain 12.2 g of the extract.

[0033] (3) Add 30mL of methanol to the extract until completely dissolved, add 30g of silica gel to mix the sample, separate by silica gel column chromatography, elute with petroleum ether-ethyl acetate solution with a volume ratio of 9:1, detect by thin layer chromatography, and collect The eluents containing betulinic acid were combined and concentrated under reduced pressure to obtain 2.77 g of crude product.

[0034] (4) Dissolve the semi-finished product in 10mL of hot me...

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Abstract

The invention discloses a method for extracting and separating betulinic acid from eleocharis tuberose peels and belongs to the field of natural organic chemistry. The method is characterized by comprising the following steps of extracting betulinic acid in eleocharis tuberose peels by using any one of a methanol aqueous solution, an ethanol aqueous solution and an acetone aqueous solution as a solvent to obtain an extract, extracting the extract with ethyl acetate, separating with silica gel column chromatography to obtain a crude product, purifying the crude product by virtue of recrystallizing to obtain a betulinic acid product in which the content of the betulinic acid is above 97%. According to the method, betulinic acid is prepared from a large number of waste eleocharis tuberose peels as raw materials, the method provides a novel approach for extracting and separating betulinic acid from a natural plant, the separation effect is good, the product is high in purity, the waste eleocharis tuberose peels are changed into treasure, the method has the advantages of easily available raw materials, rich resources, simplicity in process operation and low production cost and has broad prospects of development and production, the large-scale production can be achieved and the pharmaceutical industry needs are met.

Description

technical field [0001] The invention belongs to the field of natural organic chemistry and relates to a method for extracting and separating betulinic acid, in particular to a method for extracting and separating betulinic acid from water chestnut skin. Background technique [0002] Betulinic acid, chemically named 3β-hydroxy-lupin-20(29)-en-28-acid, also known as betulinic acid, is a colorless crystal, which is a pentacyclic three Terpenoids are widely distributed in plants such as Betula, Platanus, Rhamnaceae, Myrtaceae, Araliaceae and Lotus. Betulinic acid and its derivatives have various biological activities such as anti-tumor, anti-HIV virus and anti-inflammation, among which the anti-cancer activity is famous. According to reports, this type of compound can induce apoptosis of cancer cells, inhibit tumor growth and angiogenesis, and has selective poisoning effect on normal cells and cancer cells, showing its potential in cancer treatment, especially for malignant dar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00
CPCC07J63/008
Inventor 罗杨合何星存李行任谭韩英曾彩云
Owner 广西嘉宝食品集团有限公司
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