Method for preparing asiatic acid by asiaticoside basic hydrolysis

A technology of asiatic acid and asiaticoside, which is applied in the field of asiatic acid prepared by hydrolysis of asiaticoside base, can solve the problems of large solvent consumption, time-consuming and labor-intensive, etc., and achieve high yield and purity, simple process and low investment little effect

Inactive Publication Date: 2009-05-06
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, the preparation method of Asiatic acid is mainly directly extracted from Centella asiatica grass, and it is obtained through cumbersome separation and purification processes such as extraction and chromatography, which is time-consuming and laborious, and consumes a large amount of solvents

Method used

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  • Method for preparing asiatic acid by asiaticoside basic hydrolysis
  • Method for preparing asiatic acid by asiaticoside basic hydrolysis

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Add 1000mL of 0.1mol / L NaOH aqueous solution into a 2L three-necked flask with stirring, put it in a constant temperature water bath at 45°C, start stirring, add 5g of asiaticoside raw material in 2 batches (add the second batch after 5h of reaction), and hydrolyze for 24h; Add hydrochloric acid to the hydrolyzate, adjust the pH value to 2-4, filter after precipitation to obtain a precipitate, dry the precipitate and weigh it to obtain 2.4g; collect the dried precipitate and add 24mL ethanol to dissolve, filter, add 144mL water to the filtrate Crystallized, filtered to obtain crystals, and then vacuum-dried to obtain 1.2 g of asiatic acid product, the product was analyzed by HPLC with a mass content of 90.5% asiatic acid and a yield of 45.2%.

Embodiment 2

[0027] Add 1000mL of 0.1mol / L KOH aqueous solution into a 2L three-necked flask with stirring, put it in a constant temperature water bath at 90°C, start stirring, add 10g of asiaticoside raw material in 3 batches (the total feeding time is 30min), hydrolyze for 2h; Add hydrochloric acid to the solution, adjust the pH value to 2-4, filter after precipitation to obtain a precipitate, and weigh the precipitate to obtain 5.0g after drying; add 100mL methanol to dissolve the collected dry precipitate, filter, add 700mL water crystallization to the filtrate , obtained crystals after filtration, and then vacuum-dried the crystals to obtain 3.0 g of asiatic acid product, the product was analyzed by HPLC with a mass content of 91.5% of asiatic acid and a yield of 59.6%.

Embodiment 3

[0029] Add 0.1mol / L Na to a 2L stirred three-neck flask 2 CO 3 Put 1000mL of aqueous solution into a constant temperature water bath at 80°C, start stirring, add 15g of asiaticoside raw material in 4 batches (the total feeding time is 1.5h), and hydrolyze for 6h; add sulfuric acid to the hydrolyzate, adjust the pH value to 2-4, After the precipitation, filter to obtain a precipitate, which is weighed after drying to obtain 7.3g; collect and dry the precipitate and add 292mL of ethanol to dissolve and filter, add 2336mL of water to the filtrate to crystallize, obtain a crystal after filtration, and then pass through After vacuum drying, 4.1 g of asiatic acid product was obtained. The mass content of asiatic acid was analyzed by HPLC to be 90.8%, and the yield was 54.6%.

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Abstract

The invention discloses a method for preparing asiatic acid by basic hydrolysis of asiaticoside, which comprises the following steps: 1) adding a raw material of astiaticoside into a water solution of inorganic base in batches, and hydrolyzing the raw material at a temperature of between 45 and 90 DEG C for 1-24 hours; 2) adding acid into the hydrolysate solution, adjusting the pH value to between 2 and 4, depositing the solution, and filtrating the solution to obtain precipitate; and 3) adding the precipitate into organic solvent after drying of the precipitate, dissolving the precipitate and filtering the solvent, adding water into filtrate for crystallization, obtaining a crystal after filtration of the filtrate, and drying the crystal through vacuum so as to obtain asiatic acid products. The asiatic acid products have high yield and purity and can be used for preparing raw materials medicine or astiatic acid derivant; in addition, the method has a simple technical process and low investment, and is easy to realize industrialization.

Description

technical field [0001] The invention relates to a method for preparing asiatic acid by hydrolyzing asiaticoside. Background technique [0002] Centella asiatica (L.) Urban is a plant of the genus Centella asiatica in the Umbelliferae family. It has a long history of application in the field of traditional medicine in many countries and regions. The internal and external use of Centella asiatica in traditional Chinese medicine has been It has a history of two thousand years. Centella asiatica is bitter in the mouth, pungent, cold in nature, nontoxic, returns liver, spleen, kidney, stomach meridian. According to ancient pharmacopoeia records, it is mainly used to treat diseases such as damp-heat jaundice, heatstroke diarrhea, sand and blood, carbuncle sores, and bruises. Modern pharmacological research and application have shown that Centella asiatica can be used to treat depression, skin wounds, gastric ulcers, infectious hepatitis, skin diseases, and epidemic cerebrospinal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00A61K36/23
Inventor 吕秀阳贾广韬李音
Owner ZHEJIANG UNIV
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