A method for preparing madecassic acid by hydrolyzing madecassic acid

A technology of madecassic acid and asiatic acid, which is applied in the direction of steroidal compounds and organic chemistry, can solve the problems of time-consuming, laborious and cumbersome, and achieve the effect of simple process, high yield and purity, and low investment

Inactive Publication Date: 2012-02-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, the preparation method of madecassic acid is mainly directly extracted from Centella asiatica grass, and it is obtained through cumbersome extraction, chromatography, crystallization and other separation and purification processes, which is time-consuming and laborious

Method used

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  • A method for preparing madecassic acid by hydrolyzing madecassic acid
  • A method for preparing madecassic acid by hydrolyzing madecassic acid
  • A method for preparing madecassic acid by hydrolyzing madecassic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Add 500mL of a mixed solution of methanol, water and sulfuric acid to a 1L 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 65°C , start stirring and condensing water, add 10g madecassoside raw material, hydrolyze for 24h; hydrolyzate is concentrated under reduced pressure to remove methanol, precipitate and filter to obtain a precipitate, which is weighed to obtain 4.7g after drying; collect and dry Add 23.5mL of methanol to dissolve the precipitate, filter, add 423mL of water to the filtrate to crystallize, and obtain crystals after filtration, and then vacuum-dry the crystals to obtain 3.3g of madecassic acid product. The quality of madecassic acid is analyzed by HPLC Content 85.9%, yield 60.8%.

Embodiment 2

[0030] Add 500mL of a mixed solution of methanol, water and hydrochloric acid to a 1L 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 20g madecassoside 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 9.3g after drying; collect and dry Add 93mL of ethanol to the precipitate to dissolve, filter, add 1488mL of water to the filtrate to crystallize, obtain crystals after filtration, and then vacuum dry the crystals to obtain 6.7g of madecassic acid product, the product is analyzed by HPLC for the mass content of madecassic acid 90.6%, yield 65.1%.

Embodiment 3

[0032] Add 500mL of a mixed solution of methanol, water and sulfuric acid to a 1L three-necked flask with a stirring and water condenser, wherein the volume percentage of methanol is 30%, and the equivalent concentration of sulfuric acid is 1.0N; the three-necked flask is placed in a constant temperature water bath at 60°C , stir and condense water, add 30g madecassoside raw material, hydrolyze for 8h; hydrolyzate is concentrated under reduced pressure to remove methanol, precipitate and filter to obtain precipitate, which is weighed after drying to obtain 14.0g; collect and dry Add 210mL of ethanol to the precipitate to dissolve, filter, add 2940mL of water to the filtrate to crystallize, obtain crystals after filtration, and then vacuum dry the crystals to obtain 9.9g of madecassic acid product, the product is analyzed by HPLC for the mass content of madecassic acid 91.0%, yield 64.4%.

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Abstract

The invention discloses a method for preparing madecassic acid by hydrolyzing madecasinic acid. The steps of the method are as follows: 1) Add madecassoside raw material into the mixed solution of organic solvent I, water and inorganic acid, and hydrolyze at 45-80° C. for 1-24 hours; 2) Concentrate the hydrolyzate under reduced pressure to remove organic solvent I , filtered after precipitation to obtain a precipitate; 3) After the precipitate was dried, an organic solvent II was added to dissolve and filter, and the filtrate was added with water to crystallize, and the crystal was obtained after filtration, and the crystal was vacuum-dried to obtain a product of madecassic acid. The product yield and purity of the madecassic acid of the invention are high, and the product can be used as a raw material medicine or the preparation of madecassic acid derivatives; meanwhile, the method has a simple process, requires less investment, and is easy to realize industrialization.

Description

technical field [0001] The invention relates to a method for preparing madecassic acid by hydrolyzing madecasinic 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, 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 me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00
Inventor 吕秀阳李音贾广韬
Owner ZHEJIANG UNIV
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