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Method for producing asiatic acid with asiaticoside acid hydrolysis

A technology of asiatic acid and asiatic acid, which is applied in the direction of pharmaceutical formulas, medical preparations containing active ingredients, steroidal compounds, etc., can solve the problems of tediousness, time-consuming and labor-intensive consumption, and large solvent consumption, and achieve simple process , high yield and purity, low investment effect

Inactive Publication Date: 2009-05-13
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] 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 labor-intensive, and consumes a large amount of solvents

Method used

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  • Method for producing asiatic acid with asiaticoside acid hydrolysis
  • Method for producing asiatic acid with asiaticoside acid hydrolysis
  • Method for producing asiatic acid with asiaticoside acid hydrolysis

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Add 1000mL of a mixed solution of methanol, water and sulfuric acid to a 2L three-necked flask with a stirring and water condenser, wherein the volume percentage of methanol is 10%, and the equivalent concentration of sulfuric acid is 0.1N; the three-necked flask is placed in a constant temperature water bath at 70°C , stir and condense water, add 5g asiaticoside raw material, hydrolyze for 15h; hydrolyzate is concentrated under reduced pressure to remove methanol, precipitate and filter to obtain a precipitate, which is weighed to obtain 2.0g after drying; collect and dry The precipitate was dissolved by adding 20mL of methanol and filtered, and the filtrate was crystallized by adding 120mL of water, and the crystal was obtained after filtration, and the crystal was dried in vacuum to obtain 1.0g of Asiatic acid product, and the product was analyzed by HPLC. The mass content of Asiatic acid was 85.2%. Yield 36.8%.

Embodiment 2

[0032] Add 1000mL of a mixed solution of methanol, water and hydrochloric acid to a 2L three-necked flask with a stirring and water condenser, wherein the volume percentage of methanol is 20%, and the equivalent concentration of hydrochloric acid is 0.5N; the three-necked flask is placed in a constant temperature water bath at 65°C , start stirring and condensing water, add 6g of asiaticoside raw material, hydrolyze for 10h; hydrolyzate is concentrated under reduced pressure to remove methanol, precipitate and filter to obtain a precipitate, which is weighed to obtain 2.5g after drying; collect and dry The precipitate was dissolved by adding 50mL of ethanol, filtered, and the filtrate was crystallized by adding 350mL of water, and the crystal was obtained after filtration, and the crystal was dried in vacuum to obtain 1.6g of Asiatic acid product, and the product was analyzed by HPLC. The mass content of Asiatic acid was 90.1%. Yield 51.8%.

Embodiment 3

[0034] Add 1000mL of methanol, water and sulfuric acid mixed solution into a 2L three-necked flask with stirring and water condenser, wherein the volume percentage of methanol is 30%, and the equivalent concentration of sulfuric acid is 1N; the three-necked flask is placed in a constant temperature water bath at 60°C, Turn on stirring and condensing water, add 8g of asiaticoside raw material, and hydrolyze for 8 hours; the hydrolyzate is concentrated under reduced pressure to remove methanol, precipitated and filtered to obtain a precipitate, which is weighed after drying to obtain 3.6g; collect the dried precipitate Add 108mL of methanol to dissolve the product, filter, add 864mL of water to the filtrate to crystallize, obtain crystals after filtration, and then vacuum dry the crystals to obtain 2.2g asiatic acid product, the product is analyzed by HPLC. The mass content of asiatic acid is 91.4%. The rate is 54.2%.

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Abstract

The invention discloses a method for preparing asiatic acid by asiaticoside acid hydrolysis. The method comprises the following steps: 1) adding the asiaticoside raw material into a mixed solution of an organic solvent I, water and inorganic acid to be hydrolyzed at a temperature of between 45 and 90 DEG C for 1 to 24 hours; 2) concentrating under reduced pressure hydrolyzate to remove the organic solvent I, filtering the precipitated solvent to obtain a precipitate; and 3) adding an organic solvent II into the dried precipitate to be dissolved and filtered, adding water crystal into filtrate, filtering the mixed solvent to obtain crystal, and drying the crystal in vacuum to obtain the asiatic acid product. The asiatic acid product has high yield and purity, can be used for preparation of a bulk drug or asiatic acid derivates; meanwhile, the method has a simple technological process and small investment, and can realize industrialization easily.

Description

technical field [0001] The invention relates to a method for preparing asiatic acid by hydrolyzing asiatic acid. 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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