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Novel process for extracting diosgenin

A technology of diosgenin and a new process, which is applied in the field of extraction process of diosgenin, can solve the problems of complicated equipment, shortened reaction time, and large water consumption, so as to reduce the amount of acid used, increase the yield of saponin, reduce the The effect of water consumption

Inactive Publication Date: 2012-10-03
SHAOYANG CHANGYUAN BIO TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The existing technology uses different methods to reduce the acid consumption of the process and reduce COD emissions; for example, the use of physical methods to separate starch and cellulose. The starch and cellulose are separated by sieving and spinning, and then the remaining saponins are processed. This process can greatly reduce pollution emissions. However, because saponins mainly exist in the cell wall in the form of combining with polyhydroxy substances, mechanical and physical methods cannot avoid the separation process. entrainment situation, at the same time, the equipment investment of this method increases, and the physical process is complex and cumbersome. In order to effectively separate starch and cellulose, a large amount of water needs to be added in the process, and there are also situations of large water consumption and sewage. In addition, the method The technological method cannot effectively deal with the starch modification in dried turmeric
[0008] Chinese patent (Application No. 03127944.9) proposes a pretreatment method using ultrasonic waves, which shortens the reaction time. At the same time, the hydrolysis system after strong acid treatment is distilled, concentrated and dried, and then supercritical extraction is used to extract saponin without sewage. emissions, but this process not only requires a large investment in equipment, but also the cost of the process is too high, and the industrial value is very low
The Chinese patent (publication number CN101705275) uses surfactants and ultrasonic waves to separate starch and cellulose, and then purifies the saponin liquid through a resin column. The process is complicated, the water consumption is large, and the industrial value is very low.
[0009] Solvent extraction is a common method for extracting natural products. However, due to the low content of saponin in yam yam and the close combination with polyhydroxy substances in yam, the extraction is very complicated and the yield is low. The report of directly extracting saponin by solvent (" Journal of Wuhan Institute of Science and Technology, No. 06, 2005, Cheng Jun) shows that the yield rate is only 63.7% of the traditional craft
In the Chinese patent (publication number CN101560239), salt is used to destroy the combination of saponins and polyhydroxy substances, which improves the extraction efficiency and separation effect, and effectively reduces pollution emissions. However, this process uses a large amount of solvent extraction, and there are filter residue entrainment, repeated distillation, etc. It leads to the problem of excessive solvent loss. At the same time, the recovery process of the extraction solvent is increased, the equipment is complicated, and the energy consumption is large. In addition, the traditional process is used when processing saponins. The amount of acid used is still too large, and the waste liquid treatment is troublesome.
However, the process has the following problems: firstly, the enzymatic hydrolysis requires high conditions, and it is necessary to add water several times the amount of the material, resulting in a large amount of waste liquid treatment; the sugar-containing saponin slurry is highly viscous and difficult to separate; the enzymatic hydrolysis of cellulose is not complete, and the subsequent Increased acid consumption and pollution during acid hydrolysis

Method used

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  • Novel process for extracting diosgenin

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) Take by weighing 100 grams of fresh Dioscorea scutellaria rhizome samples that have been washed and removed;

[0034] (2) The sample is crushed, and 200 grams of water is added to make a slurry;

[0035] (3) Filter the solid-liquid mixture with double-layer gauze, add 100 grams of water to the filter residue, continue to crush it once with a Joyoung cooking machine, collect the filtrate, and collect the filter residue separately for processing;

[0036] (4) Pour the filtrate into a separatory funnel and let it stand for layers. The upper layer is a clear liquid layer, the middle is a suspension layer, and the lower white layer is a starch layer. Pour out a total of 350ml of the upper layer and the middle layer into a beaker, and collect the lower layer. Starch to be processed.

[0037] (5) Add 0.2 g of Rhodotorula viscoscens strain to the suspension, let it stand for fermentation for 24 hours, separate 250ml of the supernatant (Rhododovis viscoscens strain A), and ...

Embodiment 2

[0044] (1) Take by weighing 100 grams of fresh Dioscorea scutellaria rhizome samples that have been washed and removed;

[0045] (2) The sample is pulverized, and the Rhodotorula viscosus bacterium liquid A added in embodiment 1 is transferred into slurry;

[0046] (3) Leave to ferment for 48 hours, separate 200ml of the supernatant (Rhodotorula viscosum liquid A), and transfer 100ml of the remaining concentrated saponin mixture into the autoclave;

[0047] (4) Slowly add concentrated sulfuric acid into the suspension to adjust the concentration of sulfuric acid to 0.5N, add 1.5 g of ferric sulfate, adjust the temperature to 125°C, and hydrolyze in an autoclave for 3 hours.

[0048] (5) Filter the hydrolyzate to separate the filter residue, wash it with a small amount of lime solution and water successively until the pH value is neutral, and combine the filtrate and lotion to about 120ml.

[0049] (6) The filter residue, namely the hydrolyzate, was oven-dried at 60°C to obtai...

Embodiment 3

[0053] (1) Take by weighing 100 grams of fresh Dioscorea scutellaria rhizome samples that have been washed and removed;

[0054] (2) Pulverize the sample, add 1.2 grams of Rhodotorula viscosum and 250 milliliters of water to make a slurry;

[0055] (3) Leave to ferment for 48 hours, separate 250ml of the supernatant (Rhodotorula viscosum liquid A), and transfer 100ml of the remaining concentrated saponin mixture into the autoclave;

[0056] (4) Slowly add concentrated hydrochloric acid into the suspension to adjust the concentration of hydrochloric acid to 1.0N, add 1.5 g of ferric chloride salt, adjust the temperature to 125°C, and hydrolyze in an autoclave for 3 hours.

[0057] (5) Filter the hydrolyzate to separate the filter residue, wash it with a small amount of lime solution and water successively until the pH value is neutral, and combine the filtrate and lotion to about 120ml.

[0058] (6) The filter residue, namely the hydrolyzate, was oven-dried at 60°C to obtain 5...

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Abstract

The invention provides an extraction process of diosgenin, and particularly discloses a process for extracting saponin in yam through microbial strengthened fermentation in combination with a dilute acid catalytic hydrolysis method. The process comprises the following steps of: cleaning and crushing the yam; performing the microbial strengthened fermentation to separate the saponin from starch and cellulose; then hydrolyzing with dilute acid under the action of a catalyst to obtain the diosgenin; performing soxhlet extraction on hydrolysate by using a solvent; and finally crystallizing and drying to obtain the finished product diosgenin. The process has the advantages of simple process, short process time, less acid consumption, less wastewater, reduced COD (Chemical Oxygen Demand) in the wastewater, extreme easiness in treatment and capability of effectively reducing the cost and the pollution.

Description

technical field [0001] The invention relates to a process for extracting diosgenin, in particular to a process for extracting dioscin in diosgenin through enhanced fermentation by microorganisms combined with dilute acid catalyzed hydrolysis. Background technique [0002] The raw material of saponin to prepare steroid hormone drugs can only be obtained from plants through a certain process. Among them, the most basic and ideal intermediate for the preparation of steroid hormone drugs is diosgenin, and diosgenin is used as the basis 67% of the world's steroid hormone drugs are produced with it as a raw material. In order to enhance our country's international competitiveness, it is imperative to improve and innovate the backward production technology of diosgenin. [0003] The scientific name of turmeric is Dioscorea shield leaf, (in the following description, the common name is often used as turmeric). It is widely planted in the Qinling Mountains and the upper and middle r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J71/00
Inventor 曾清如
Owner SHAOYANG CHANGYUAN BIO TECH
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