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Method of finely extracting ursolic acid from haw

A technology of ursolic acid and hawthorn, which is applied in the direction of steroids and organic chemistry, can solve the problems of unstable yield, high process requirements, and difficult process control, and achieve an easy-to-achieve effect

Active Publication Date: 2012-12-26
WUHAN LIYUANHENG PHARMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method adopts alkaline dissolution, reuses acidic precipitation, and requires PH3~4, and process requirement is high, through repeated tests by the inventor, said method can only be applicable to the small test of laboratory, when carrying out large-scale industrialized production, Due to the difficulty of process control, the product quality, purity and yield are unstable, so it is not suitable for the production of pharmaceutical raw materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Boil the sample to remove most of the water solubility; take 10 kg of hawthorn and add water 5 times the weight of the hawthorn; after boiling the water, keep it at 70°C for 0.5 hours, and dry the filter residue at 70°C after suction filtration .

[0019] (2) Take the product dried in step (1) and use the volume concentration of 6 times the weight of the product to be 95% ethanol for reflux extraction once for 4 hours, and recover under reduced pressure to dry extract and no alcohol smell, the specific gravity of dry extract Control between 0.85 ~ 1.30g / ml.

[0020] (3) disperse the dry extract with 70°C water of 5 times the weight of the dry extract,

[0021] Adjust the pH value to 11.5 with sodium hydroxide, place the first precipitate, suction filter, wash the precipitate with distilled water until the pH of the precipitate filtrate is equal to 7, obtain the second precipitate, and filter the second precipitate at 70 Dry at ℃ for later use.

[0022] (4) Take t...

Embodiment 2

[0027] (1) Take 50 kg of hawthorn and add water 10 times the weight of the hawthorn; boil the water and keep it at 80°C for 1.5 hours, and dry the filter residue at 70°C after suction filtration.

[0028] (2) get the product that step (1) dries and use the volume concentration of this product 3 times of weight parts to be 95% ethanol reflux extraction 2 times, the weight of reflux extraction ethanol for the first time is 6 times of product weight; Time 3 hours ; The weight of the second reflux extraction of ethanol is 5 times the weight of the product; the time is 1h, the extract is combined; the dry extract is recovered under reduced pressure and has no alcohol smell, and the specific gravity of the dry extract is controlled between 0.85 ~ 1.30g / ml .

[0029] (3) disperse the dry extract with 70°C water of 10 times the weight of the dry extract,

[0030] Adjust the pH value to 12 with sodium hydroxide, place the first precipitate, suction filter, wash the precipitate with di...

Embodiment 3

[0036] (1) Take 100 kg of hawthorn and add water 30 times the weight of the hawthorn; boil the water and keep it at 70°C for 3 hours, and dry the filter residue at 70°C after suction filtration.

[0037] (2) get the product that step (1) dries and use the volume concentration of 8 times of weight parts of this product to be 50~100% ethanol reflux extraction 3 times, the weight of reflux extraction ethanol for the first time is 6 times of product weight; Time 1.5 hours; the weight of ethanol extracted by reflux for the second time is 5 times of the weight of the product; time 1.5h, the weight of ethanol extracted by reflux for the third time is 4 times of the weight of the product; time 1h, combined extracts; reduced pressure recovery to The dry extract has no alcohol smell, and the specific gravity of the dry extract is controlled between 0.85-1.30g / ml.

[0038] (3) disperse the dry extract with 70°C water of 40 times the weight of the dry extract,

[0039] Adjust the pH valu...

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PUM

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Abstract

The invention discloses a method of finely extracting ursolic acid from haws. Water-soluble impurities are removed after haws being boiled in water. Then the haws are extracted and concentrated by ethyl alcohol reflux. The PH value of reconcentrate is adjusted to alkaline to obtain the sediments. Flush the sediments with water till to neutral. Ursolic acid is obtained after the sediments being decoloured and recrystallized. The method is suitable for industrial production of ursolic acid in large scale.

Description

technical field [0001] The invention belongs to the extraction of ursolic acid, in particular to a method for finely extracting ursolic acid from hawthorn. Background technique [0002] Ursolic acid (Ursolic acid), also known as ursolic acid and ursolic acid, is a pentacyclic triterpene acid. In vitro tests show that this product is effective against human colon cancer cells (HCT-8), human cervical cancer cells (Hela), human Melanoma cells (MV3), human gastric cancer cells (BGC-823), human giant cell lung cancer cells (801-D), human ovarian cancer cells (A2780), human oral epithelial cancer cells (KB), etc. have obvious inhibitory effect ;Tumor-bearing mice test results show that this product has a significant inhibitory effect on human transplanted liver cancer (Bel-7402), human liver cancer (SMMC-7721), mouse Lewis lung cancer (3LL), S180, and H22. Ursolic acid can directly kill tumor cells by activating RARP and endonucleases in cancer cells to attack nuclear and nucleos...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00
Inventor 张长弓易以木白岩
Owner WUHAN LIYUANHENG PHARMA TECH
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