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Method for purifying ganoderic acid T and ganoderic acid Me based on chemical synthesis method

A technology of chemical synthesis and purification method, which is applied in the field of purification of ganoderma acid T and ganoderma acid Me, can solve the problems of expensive equipment, limited enlargement prospect, unsuitability for industrialized large-scale production, etc., and achieve simplification of separation difficulty, enhancement of separation efficiency, The effect of convenient promotion

Active Publication Date: 2010-09-29
TAIXING DONGSHENG FOOD TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually, there are dozens of ganoderma acids with similar structures in the crude extract of ganoderma lucidum cells, and the contents of these substances are not much different, which causes great inconvenience to the preparative separation
Even though some high-content ganoderma acids, such as 7-ethoxy ganoderma acid O, have a preliminary large-scale separation and purification scheme CN200910308432.8, but due to the complexity of ganoderma acids in the crude extract, the prospects for the enlargement of this process limited
At the same time, there are also a large number of ganoderma acids with similar structures in the waste eluent of this kind of ganoderma acid separation and purification. These valuable wastes are difficult to be utilized by the current ganoderma acid separation process
Now, with the development and application of modern preparation and separation instruments such as preparative liquid chromatography and high-speed countercurrent chromatography, the column efficiency separation that can be achieved by preparative separation has been significantly improved, but it still cannot completely solve the problem of extracting liquids from Chinese herbal medicines. The problem of separating a single active active ingredient in a complex system, not to mention that these equipment are expensive and not suitable for large-scale industrial production

Method used

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  • Method for purifying ganoderic acid T and ganoderic acid Me based on chemical synthesis method
  • Method for purifying ganoderic acid T and ganoderic acid Me based on chemical synthesis method
  • Method for purifying ganoderic acid T and ganoderic acid Me based on chemical synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] 1. Weigh 100g of stem cell powder fermented from Ganoderma lucidum mycelium, add 1L of ethyl acetate, extract terpenoids from Ganoderma lucidum stem cells, make Ganoderma lucidum cell crude extract, and use a rotary evaporator to concentrate it into an extract , Obtain 10.3 g of extract-like substance. HPLC analysis such as figure 1 , which contains 0.52g of ganoderma acid T and 0.3g of ganoderma acid Me.

[0052] 2. Redissolve the extract of Ganoderma lucidum cells in 1L of dichloromethane, add 50mL of acetic anhydride and 3g of DMAP as a catalyst, and carry out the acetylation reaction in a water bath at 40°C for 8 hours. After the reaction, the catalyst DMAP and unreacted acetic anhydride in the reaction system were extracted with 500 mL of HCl solution with a hydrogen ion concentration of 0.06 mol / L. After liquid separation, the aqueous phase containing DMAP was used to recover DMAP, and the organic phase containing ganoderma acid was processed by rotary evaporati...

Embodiment 2

[0056] 1. Weigh 100g of stem cell powder fermented from Ganoderma lucidum mycelium, add 1L of ethyl acetate, extract terpenoids from Ganoderma lucidum stem cells, make Ganoderma lucidum cell crude extract, and use a rotary evaporator to concentrate it into an extract , Obtain 10.3 g of extract-like substance. HPLC analysis such as figure 1 , which contains 0.52g of ganoderma acid T and 0.3g of ganoderma acid Me.

[0057] 2. Redissolve the Ganoderma lucidum cell extract in 1L of dichloromethane, add 50mL of acetic anhydride and 4ml of pyridine as a catalyst, and carry out the acetylation reaction in a water bath at 40°C for 8 hours. After the reaction, the catalyst DMAP and unreacted acetic anhydride in the reaction system were extracted with 500 mL of HCl solution with a hydrogen ion concentration of 0.06 mol / L. After liquid separation, the aqueous phase containing DMAP was used to recover DMAP, and the organic phase containing ganoderma acid was processed by rotary evaporat...

Embodiment 3

[0061] 1. Weigh 100g of stem cell powder fermented from Ganoderma lucidum mycelium, add 1L of ethyl acetate, extract terpenoids from Ganoderma lucidum stem cells, make Ganoderma lucidum cell crude extract, and use a rotary evaporator to concentrate it into an extract , Obtain 10.3 g of extract-like substance. HPLC analysis such as figure 1 , which contains 0.52g of ganoderma acid T and 0.3g of ganoderma acid Me.

[0062] 2. Redissolve the Ganoderma lucidum cell extract in 1L of dichloromethane, add 50mL of acetic anhydride and 0.3g of DMAP as a catalyst, and carry out the acetylation reaction in a water bath at 40°C for 8 hours. After the reaction, the catalyst DMAP and unreacted acetic anhydride in the reaction system were extracted with 500 mL of HCl solution with a hydrogen ion concentration of 0.06 mol / L. After liquid separation, the aqueous phase containing DMAP was used to recover DMAP, and the organic phase containing ganoderma acid was processed by rotary evaporation...

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Abstract

The invention relates to a method for purifying ganoderic acid T and ganoderic acid Me based on a chemical synthesis method, belonging to the technical field of extraction of traditional Chinese medicines. The method comprises the following steps of: concentrating a ganoderic acid crude extract to extractum-shaped ganoderma cell extract extractum through rotary evaporator treatment, then dissolving the ganoderma cell extract extractum to an organic solvent and adding an acetylation reagent, carrying out acetylation reaction under the monitoring of reversed phase liquid chromatography, extracting the acetylation reagent by utilizing a neutralizer, concentrating ganoderma cell extract after acetylation to form an extractum shape through the rotary evaporator treatment, renewedly dissolving the ganoderma cell extract to a mixed system of carbinol or carbinol and water, adding an acid catalyst for carrying out acid catalyzed reaction under the monitoring of the reversed phase liquid chromatography, and finally placing neutralized acid catalytic reaction products in a rotary evaporator for volatilizing to dryness to obtain ganoderic acid crude products with more than 45% of ganoderic acid T and more than 25% of ganoderic acid Me.

Description

technical field [0001] The invention relates to a method in the technical field of preparation of traditional Chinese medicines, in particular to a method for purifying ganoderma acid T and ganoderma acid Me based on a chemical synthesis method. Background technique [0002] Ganoderma lucidum, as a precious medicinal material, has a long history of medicinal use in China and Southeast Asia. Modern medical research shows that Ganoderma acid is one of the important active ingredients of Ganoderma lucidum, which has pharmacological functions such as anti-cancer, anti-HIV virus, and anti-inflammatory response. Acta.Pharmacol.Sin., 25(11), 1387-1395, 2004. Recently, a number of first-line research groups in the world have successively reported the anticancer efficacy and related anticancer mechanism of monomeric ganoderma acid, such as ganoderma acid D and X, Molecule & Cell Proteomics, 7(5), 949-961, 2007; Life Sciences 77(3), pp. 252-265. Other prior art also shows that Ganod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 钟建江王家乐秦汉林
Owner TAIXING DONGSHENG FOOD TECH
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