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Method for preparing diosgenin from B acid DES (deep eutectic solvent) hydrolysis

A technology of diosgenin and B acid, which is applied in the direction of chemical instruments and methods, steroids, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problems of diosgenin polluting the environment and achieve flexible equipment technology , and the effect of good economy and simple raw material processing

Active Publication Date: 2018-08-03
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But there is the problem of serious environmental pollution when this method produces diosgenin

Method used

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  • Method for preparing diosgenin from B acid DES (deep eutectic solvent) hydrolysis
  • Method for preparing diosgenin from B acid DES (deep eutectic solvent) hydrolysis
  • Method for preparing diosgenin from B acid DES (deep eutectic solvent) hydrolysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) heating choline chloride and citric acid according to the molar ratio of 2:1 to 69°C and melting to obtain DES;

[0027] (2) Add 5g of Dioscorea baicalensis underground rhizome raw material powder, 100ml of DES and 100ml of petroleum ether (boiling range is 90-120) into a 250ml round bottom flask, so that petroleum ether and DES form a two-phase solvent system;

[0028] (3) Set up the condensing reflux device. Turn on the condensed water and oil bath heating switches, and set the reaction temperature to 110°C. After the temperature was raised to 100°C, the hydrolysis reaction was carried out at a constant temperature for 4 hours. After the reaction is terminated, turn off the condensate water and the heating switch, take out the flask and wait for it to cool to normal temperature. The reaction solution is separated with a Buchner funnel, and the liquid petroleum ether phase rich in diosgenin is taken; the solid phase residue is washed three times with petroleum et...

Embodiment 2

[0032] (1) heating choline chloride and oxalic acid according to the molar ratio of 1:1 to 60°C and melting to obtain DES;

[0033] (2) Add 3g of Dioscorea baicalensis underground rhizome raw material powder, 60ml of DES and 60ml of petroleum ether (boiling range is 90 to 120) into a 150ml round bottom flask, so that petroleum ether and DES form a two-phase solvent system;

[0034] (3) Set up the condensing reflux device. Turn on the condensed water and oil bath heating switches, and set the reaction temperature to 100°C. After the temperature was raised to 110°C, the hydrolysis reaction was performed at a constant temperature for 4 hours. After the reaction is terminated, turn off the condensate water and the heating switch, take out the flask and wait for it to cool to normal temperature. The reaction solution is separated with a Buchner funnel, and the liquid petroleum ether phase rich in diosgenin is taken; the solid phase residue is washed three times with petroleum eth...

Embodiment 3

[0039] (1) Heating choline chloride and succinic acid in a molar ratio of 1:1 to 71°C to melt to obtain DES;

[0040] (2) Add 10g of Dioscorea baicalensis underground rhizome raw material powder, 200ml of DES and 200ml of petroleum ether (boiling range is 90-120) into a 150ml round bottom flask, so that petroleum ether and DES form a two-way solvent system;

[0041] (3) Set up the condensing reflux device. Turn on the condensed water and oil bath heating switches, and set the reaction temperature to 130°C. After the temperature was raised to 130°C, the hydrolysis reaction was performed at a constant temperature for 2 hours. After the reaction is terminated, turn off the condensate water and the heating switch, take out the flask and wait for it to cool to normal temperature. The reaction solution is separated with a Buchner funnel, and the liquid petroleum ether phase rich in diosgenin is taken; the solid phase residue is washed three times with petroleum ether (boiling rang...

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Abstract

The invention belongs to the technical field of plant ingredient extraction, and discloses a method for preparing diosgenin from B acid DES (deep eutectic solvent) hydrolysis. Choline chloride and B acid are heated to a molten state so as to obtain a DES; dioscorea zingiberensis rhizome raw material powder, the DES and petroleum ether are added into a reactor; the temperature is raised to 100 to 130 DEG C; stirring and hydrolysis reaction are preformed; reaction liquid is subjected to filtering or centrifugal separation; a liquid petroleum ether phase is taken; petroleum ether recovered through evaporation; the diosgenin in the rest solid phase is extracted by using water saturation normal butanol solution; the normal butanol and the water are recovered through evaporation; the diosgenin is obtained. The characteristic that the B acid DES and the diosgenin can form strong hydrogen bonds is utilized, so that the DES can realize the selective extraction of the diosgenin from the raw materials for hydrolysis. The method has the advantages that the reaction selectivity is good; the pollution is low; the reaction conditions are mild; the problem of high pollution caused by simultaneoushydrolysis of cellulose and starch in the raw materials into sugar in a conventional hydrolysis process can be solved.

Description

technical field [0001] The invention belongs to the technical field of plant component extraction, and in particular relates to a method for preparing diosgenin by hydrolysis of B acid DES. Background technique [0002] Dioscorea zingiberensis C.H.Wright, a plant of the genus Dioscorea zingiberensis, is an important medicinal and edible resource. The underground rhizome of Dioscorea thunifolius has very high medicinal value, and it has been included in the Compendium of Materia Medica since ancient times. Modern natural product research shows that the steroidal saponin contained in the rhizome of Dioscorea shield leaf is its main active substance, which has the effects of lowering blood pressure, lowering blood fat, anti-inflammatory and anti-cancer. Because steroidal sapogenins have such good efficacy, it is necessary to develop a large-scale production process of sapogenins. [0003] At present, the main method for preparing diosgenin is acid hydrolysis. That is to firs...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J71/00B01J31/02
CPCB01J31/0239C07J71/0005
Inventor 付严向程张涛邱浩新刘家俊徐亚飞
Owner SOUTH CHINA UNIV OF TECH
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