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Preparation method of hederagenin

A technology of helexin and acid hydrolysis, applied in steroids, organic chemistry and other directions, can solve the problems of polluted aglycon content and transfer rate, unfavorable to industrialized production, complicated steps, etc.

Active Publication Date: 2012-10-03
杨中林
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is complicated in steps, and a large amount of organic solvents are used, which is easy to cause pollution and the aglycon content and transfer rate are poor; Xin Xuelei et al. prepared normal Idygenin, the method adopts multiple organic solvents, which is unfavorable for suitability for industrialized production

Method used

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  • Preparation method of hederagenin
  • Preparation method of hederagenin
  • Preparation method of hederagenin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0103] Soak the coarse powder of Dipsacus officinalis through a 40-mesh sieve (with a content of 4% aketoside D) in 90% ethanol for 2 hours, heat and reflux for extraction three times, the amount of ethanol is 30 times the weight of Dipsacus, and the extraction time is A total of 6 hours, 2 hours each time, combined the extracts 3 times, and filtered; the filtrate recovered ethanol until it had no alcohol smell to obtain a crude extract, the yield of the crude extract was about 6%, and the transfer rate of aketoside D was 98%;

[0104] Add ethanol and hydrochloric acid with a concentration of 95% to the crude extract, stir well, and obtain an acidolysis solution, so that the volume fraction of hydrochloric acid in the acidolysis solution is 7%, the volume fraction of ethanol is 50%, and the acidolysis temperature is 80 ° C. The solution time is 4h, and the ratio of solid to liquid is 1:30. The solution obtained after acid hydrolysis was recovered from ethanol until it had no ...

Embodiment 2

[0106] Soak the coarse powder of Dipsacus officinalis through a 40-mesh sieve (the content of Akebia saponin D is 4%) in 90% ethanol for 2 hours, and heat and reflux for extraction three times. A total of 6 hours, 2 hours each time, combined the extracts 3 times, and filtered; the filtrate recovered ethanol until it had no alcohol smell to obtain a crude extract, the yield of the crude extract was about 6%, and the transfer rate of aketoside D was 97.5%;

[0107] Add ethanol and hydrochloric acid with a concentration of 95% to the crude extract, stir well, and obtain an acidolysis solution, so that the volume fraction of hydrochloric acid in the acidolysis solution is 9%, the volume fraction of ethanol is 50%, and the acidolysis temperature is 80°C. The solution time is 4h, and the ratio of solid to liquid is 1:50. The solution obtained after acid hydrolysis was recovered from ethanol until it had no alcohol smell, allowed to cool at room temperature, precipitated, filtered t...

Embodiment 3

[0109] Soak the coarse powder of Dipsacus officinalis through a 40-mesh sieve (with a content of 4% aketoside D) in 80% ethanol for 2 hours, heat and reflux for extraction twice, the amount of ethanol is 18 times the weight of Dipsacus, and the extraction time is A total of 9 hours, 4.5 hours each time, combined 2 extracts, filtered; the filtrate recovered ethanol until it had no alcohol smell to obtain a crude extract, the yield of the crude extract was about 6%, and the transfer rate of aketoside D was 97% ;

[0110]Add ethanol and hydrochloric acid with a concentration of 95% to the crude extract, stir well, and obtain an acidolysis solution, so that the volume fraction of hydrochloric acid in the acidolysis solution is 5%, the volume fraction of ethanol is 50%, and the acidolysis temperature is 65 ° C. The solution time is 6h, and the ratio of solid to liquid is 1:40. The solution obtained after acid hydrolysis was recovered from ethanol until it had no alcohol smell, all...

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Abstract

The invention discloses a preparation method of hederagenin. The method comprises the following steps of: performing alcohol extraction on teasel root medicinal material and then performing acidolysis; concentrating solution obtained by the acidolysis; standing and cooling; and filtering to obtain precipitate which is the hederagenin. The extraction method of the hederagenin is simple and convenient and has high transfer rate, the purity of the obtained hederagenin is over 93 percent, and the extraction method is pollution-free and is easy for industrial production.

Description

technical field [0001] The invention belongs to the technical field of traditional Chinese medicines, and in particular relates to a preparation method of hedera saponin. Background technique [0002] Hederagenin (Hederagenin), alias (3beta, 4alpha)-3,23-Dihydroxyolean-12-en-28-oicacid; hederagenin, molecular formula C 30 h 48 o 4 , can be obtained from the market or prepared by various ways, taste bitter, hygroscopic, stimulate mucous membranes, soluble in water, easily soluble in hot water, hot methanol and hot ethanol, insoluble in ether, etc. of organic solvents. The molecular structure is as follows: [0003] [0004] Wu Yaomin et al. hydrolyzed the saponin with acid from the seed of Prechia, filtered it, washed the insoluble matter of the filtrate with water to remove excess acid, and then drained it to obtain the crude product. For further purification, use medicinal ethanol to heat to dissolve the coarse crystals, add activated carbon to decolorize, heat to r...

Claims

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Application Information

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IPC IPC(8): C07J63/00
Inventor 杨中林
Owner 杨中林