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Green process for preparing diosgenin

A technology of diosgenin and green technology, applied in the direction of steroids, organic chemistry, etc., can solve the problems of reducing saponin quality, increasing uncertainty expectations, and low cost, so as to simplify subsequent processes and improve saponin quality , The effect of low extraction cost

Inactive Publication Date: 2015-07-01
DALIAN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are three major defects in this type of method: 1. Microorganisms may destroy part of saponin, so its saponin increase is not significant; 2. The introduction of microbial secondary metabolic impurities reduces the quality of saponin; 3. Fermentation products are not dioscin Elements have become the main industry, introducing new competitive risks, and the uncertainty of enterprises is expected to increase
[0013] In summary, the currently disclosed methods have not yet fully met the four standards of high purity, high yield, low cost, and cleanliness. The relatively perfect natural fermentation-total glycoside alcohol extraction-acid hydrolysis method still needs to further improve the yield of saponin , quality, cost reduction and comprehensive utilization of acid hydrolyzate (recovery of acid and sugar)

Method used

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  • Green process for preparing diosgenin

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Wash 2000g of yam yam fresh material and remove the shavings, then finely grind it with 3 sets of colloid mills used in series to make a slurry, and keep it at 25°C for 48 hours for natural fermentation; after natural fermentation, the slurry is 5 times the quality of the slurry after natural fermentation Water and 3% light gasoline are fed into the colloid mill synchronously for grinding. In order to make the grinding fully, three colloid mills are used in series at the same time; after that, cellulose, starch, supernatant and emulsion are separated by centrifugation. ; Add 2M H in the ratio of acid:emulsion=1:1 2 SO 4 , and stirred and hydrolyzed at 30°C and 1 atmosphere for 6 hours, the hydrolyzate was filtered to obtain dregs, neutralized with ammonia water and washed with 10L of water, 3L of 70% ethanol was added to the dregs to extract diosgenin, the extract was filtered to remove dregs and concentrated to 300ml , refined, crystallized, and 15.94g of diosgenin wi...

Embodiment 2

[0032] Wash 500g of the dry material of Dioscorea chinensis to remove the shavings, and then fully swell it in water. It is finely ground by 4 colloid mills used in series to make a slurry, and it is kept at 30°C for 24 hours for natural fermentation; after natural fermentation, the slurry is 10 times more natural. Water of slurry quality after fermentation and the mixed solution of 5% n-hexane and heptane are synchronously fed into the colloid mill for grinding, and in order to make the grinding fully, 4 colloid mills are used in series at the same time; afterward, by centrifugation, the cellulose, 4 parts of starch, supernatant and emulsion; 2M HCl was added to the ratio of acid:emulsion = 5:1, stirred and hydrolyzed at 30°C and 1 atmosphere for 3 hours, the hydrolyzate was filtered to obtain dregs, ammonia water And, after washing with 10L of water, add 3L of 70% ethanol to the dregs to extract diosgenin, filter the dregs, concentrate to 300ml, refine, crystallize, and obtai...

Embodiment 3

[0034] Wash and remove shavings of 500g pangosaurus dry material, swell fully in water, finely grind it with 5 sets of colloid mills used in series to make a slurry, and keep it at 27°C for 40 hours for natural fermentation; after natural fermentation, the slurry is 8 times after natural fermentation Slurry quality water and 1% mixed solution composed of glyceryl monostearate, Span-60 and tween-40 are synchronously fed into the colloid mill for grinding. In order to make the grinding fully, 5 colloid mills are used in series at the same time; According to the method, 4 parts of cellulose, starch, supernatant and emulsion are separated; wherein 2M H 3 PO 4 , and stirred and hydrolyzed at 30°C and 1 atmosphere for 4 hours, the hydrolyzate was filtered to obtain dregs, neutralized with ammonia water and washed with 10L of water, 3L of 70% ethanol was added to the dregs to extract diosgenin, the extract was filtered to remove dregs and concentrated to 300ml , refined, crystallize...

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Abstract

The invention discloses a green process for preparing diosgenin and belongs to the technical field of natural product extraction. The main procedure of the process comprises the steps of washing, smashing, naturally fermenting, emulsifying, separating fibers, separating starch, separating emulsion, performing acidolysis, separating oil and water, performing reduced-pressure condensing, and recrystallizing to get the product; recovering acid and monosaccharide in the acidolysis solution through a simulated moving bed; and adding a nonpolar solvent into a natural fermentation solution while grinding by a colloid mill, emulsifying the diosgenin to form the emulsion fixed in the water, and separating to get the cellulose, starch, supernate and emulsion after emulsifying. The emulsion is directly acidolysis processed so that the hydrolysis condition is reduced, the diosgenin is free of being damaged, and the quality of the diosgenin is increased; the pollution source is completely eliminated by the acid and the monosaccharide in the acidolysis solution. The process meets the standards of high purity, high yield, low cost and pollution free. The prepared diosgenin content is greater than 98%, the yield is greater than 80%, the recovery rate of the cellulose, the starch and the like is greater than 95%, the production cost is reduced by 30%, the ton cost is reduced by **-** and no pollution is discharged.

Description

technical field [0001] The invention relates to a green process for preparing diosgenin, which belongs to the technical field of natural product extraction. Background technique [0002] The hydrolyzed product of diosgenin, diosgenin, is the basic raw material for the synthesis of more than 60 kinds of steroid hormones and contraceptive drugs, and the latter is an indispensable basic drug for modern medicine, constituting the second largest class of drugs after antibiotics. The international demand for high-quality diosgenin has been stable at about 1,000-1,200 tons (equivalent to about 8,000-9,000 tons of crude product). 75% of diosgenin is derived from dioscin, and my country has resources of dioscens scutellaria, and the output of diosgenin ranks first in the world for many years. In recent years, the monopoly position of Chinese saponin in the international market has been seriously threatened. First of all, the price of diosgenin in my country is far lower than th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J71/00
CPCC07J71/0005
Inventor 朱靖博何克江耿慧琴杨春月丁燕寇自农
Owner DALIAN POLYTECHNIC UNIVERSITY
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