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Method for preparation of Cycloastragenol by sulfuric acid hydrolysis

A technology of hydrolysis of cycloastragenol and sulfuric acid, which is applied in the field of medicine and chemical industry, and can solve the problems of complex operation, cumbersome steps, and low yield

Inactive Publication Date: 2015-08-05
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are few reports on the preparation method of cycloastragenol. The Chinese invention patent application with application number 201410101515.0 discloses a preparation method and application of cycloastragenol. , hydrolysis, extraction, and purification methods to obtain high-purity cycloastragenol products. This method can obtain cycloastragenol products with good quality, but the steps are cumbersome, the operation is complicated, and the yield is low.

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  • Method for preparation of Cycloastragenol by sulfuric acid hydrolysis

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Effect test

Embodiment 1

[0018] Preparation of crude extract of astragaloside IV: After pulverizing the traditional Chinese medicine Astragalus, take 10g of Astragalus and add it to methanol with a solid-liquid mass ratio of 1:10, then add 2% ammonia water with a mass fraction of 28% according to the mass ratio of methanol, and place in a flask The rotor was magnetically stirred, and the temperature was set at 65°C. When the first drop of condensate appeared on the condenser, the timing was started. The time for one reflux was set to 2h, and each sample was refluxed twice for extraction. After refluxing and filtering, the filtrate was spin-dried to obtain the crude extract of astragaloside IV, and the purity of astragaloside IV was 0.28% as measured by HPLC.

[0019] Preparation of cycloastragenol by acid hydrolysis: Accurately weigh 5.00 g of the crude extract of astragaloside IV, add it to 50 ml of 5% sulfuric acid solution, and react in a closed reaction kettle at 130° C. for 6 h. After the reactio...

Embodiment 2

[0022] Preparation of crude extract of astragaloside IV: Take 10 g of astragalus powder and add it to methanol with a solid-liquid mass ratio of 1:10, at a temperature of 65° C., add methanol with a mass fraction of 2% and ammonia water with a mass fraction of 28%, and place a rotor in the flask for Magnetic stirring, start timing when the first drop of condensate appears on the condenser, the time of one reflux is set to 2h, and each sample is refluxed twice for extraction. After refluxing and filtering, the filtrate was spin-dried to obtain the crude extract of astragaloside IV, and the purity of astragaloside IV was 0.31% as measured by HPLC.

[0023] Preparation of cycloastragenol by acid hydrolysis: take 5.00 g of the crude extract of glycosides, add 50 ml of sulfuric acid solution with a mass fraction of 5%, and react in a closed reaction kettle at 130°C for 6 hours. After the reaction is completed, use a mass fraction of 10% of ammonia for neutralization. Take out the ...

Embodiment 3

[0026] Preparation of the crude extract of astragaloside IV: take 100 g of astragalus powder and extract it under reflux with methanol, the mass ratio of solid to liquid is 1:10, add 2% by mass of ammonia water with a mass fraction of 28%, the temperature is 65°C, and carry out magnetic stirring. The time was set to 2h, and reflux was performed twice. After filtration, the filtrate was rotary evaporated to obtain the crude extract of glycoside A, and the purity of glycoside A was 0.25% as measured by HPLC.

[0027] Preparation of cycloastragenol by acid hydrolysis: weigh 20.00 g of the crude extract of glycoside A, add 200 ml of sulfuric acid solution with a mass fraction of 5% in a closed reaction kettle, and react at 130° C. for 6 hours. After the reaction, neutralize with 10% ammonia water. Take out the material in the kettle and place it in a beaker, add 200ml of chloroform, shake well and let it stand to remove impurities in the chloroform layer. Add 200ml of n-butanol,...

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Abstract

The invention relates to a method for preparation of Cycloastragenol by sulfuric acid hydrolysis. The method provided by the invention utilizes sulfuric acid to hydrolyze the Chinese medicine astragalus crude extract astragaloside, and realizes conversion of astragaloside to Cycloastragenol under certain hydrolysis condition, then performs impurity separation on the Cycloastragenol crude extract obtained by acid hydrolysis by chloroform and n-butanol extraction, and further makes use of silica gel column chromatography purification to finally obtain high purity Cycloastragenol. The invention aims to provide the method that can overcome the disadvantages of complex production process, low yield, high cost and the like of Cycloastragenol production and is suitable for large-scale production of different purity Cycloastragenol.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and relates to a new method for preparing cycloastragenol by hydrolyzing sulfuric acid with traditional Chinese medicine astragalus as a raw material. Background technique [0002] The active ingredients in Astragalus include flavonoids, saponins, polysaccharides and amino acids. Among them, astragaloside has the effects of strengthening the heart, lowering blood pressure, anti-tumor, lowering blood sugar in diabetic rats, and promoting insulin secretion. Dozens of astragalosides have been isolated and identified from Astragalus root, and astragaloside IV is the main active ingredient of saponins. Cycloastragenol belongs to triterpenoid saponins and is mainly obtained by hydrolysis of Astragaloside IV. Cycloastragenol is the only telomerase activator discovered today, which delays the shortening of telomeres by increasing telomerase, and cycloastragenol is considered to have anti-a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J53/00
CPCC07J53/004
Inventor 袁其朋王立媛
Owner BEIJING UNIV OF CHEM TECH
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