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Alcohol-free extraction method for dioscin

A diosgenin and extraction technology is applied in the field of alcohol-free extraction of dioscin, can solve problems such as diosgenin pollution, and achieves the effects of low cost, low extraction cost and increased protein content

Active Publication Date: 2012-05-02
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The present invention aims to provide an alcohol-free extraction method for diosgenin that can solve the problem of diosgenin pollution and reduce the production cost of diosgenin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) First, the dried Dioscorea scutellaria (Turmeric) is pulverized into 40 mesh-80 mesh diosminum scutellaria powder;

[0029] 2) Next, get 1Kg pulverized Dioscorea scutellaria powder in parts by mass and add it to 10Kg of purified water, then add OP-10 (condensate of alkylphenol and oxirane) to it to make OP-10 The mass concentration is 1.5%, after ultrasonication for 40min at a frequency of 25.8KHz, vacuum filtration is performed, and the filtrate is collected;

[0030] 3) Vacuum concentrate the filtrate to a paste at 52°C with a vacuum degree of 0.093Mpa;

[0031] 4) Take the paste concentrated in step 3) and add it to 1.5 times the mass of 1.5mol / L sulfuric acid solution for hydrolysis at 102°C. After hydrolysis, use NaOH to neutralize, wash with water, and dry the filter residue;

[0032] 5) Wrap the filter residue with filter paper and put it into a Soxhlet extractor, add petroleum ether according to the mass ratio of filter residue:petroleum ether of 1:100, heat...

Embodiment 2

[0034] 1) First, the dried Dioscorea scutellaria (Turmeric) is pulverized into 40 mesh-80 mesh diosminum scutellaria powder;

[0035] 2) Next, get 1Kg pulverized Dioscorea scutellaria powder in parts by mass and add it to 10Kg of purified water, then add OP-10 (condensate of alkylphenol and oxirane) to it to make OP-10 The mass concentration is 1.5%, after ultrasonication for 40min at a frequency of 25.8KHz, vacuum filtration is performed, and the filtrate is collected;

[0036] 3) Vacuum concentrate the filtrate to a paste at 52°C with a vacuum degree of 0.093Mpa;

[0037]4) Take the paste concentrated in step 3) and add it to 2.0 mol / L sulfuric acid solution of 3.0 times the mass for hydrolysis at 106°C. After hydrolysis, neutralize with NaOH, wash with water, and dry the filter residue;

[0038] 5) Wrap the filter residue with filter paper and put it into a Soxhlet extractor, add gasoline according to the mass ratio of filter residue: gasoline of 1:100, heat and reflux for...

Embodiment 3

[0040] 1) First, the dried Dioscorea scutellaria (Turmeric) is pulverized into 40 mesh-80 mesh diosminum scutellaria powder;

[0041] 2) Next, get 1Kg pulverized Dioscorea scutellaria powder in parts by mass and add it to 10Kg of purified water, then add OP-10 (condensate of alkylphenol and oxirane) to it to make OP-10 The mass concentration is 1.5%, after ultrasonication for 40min at a frequency of 25.8KHz, vacuum filtration is performed, and the filtrate is collected;

[0042] 3) Vacuum concentrate the filtrate to a paste at 52°C with a vacuum degree of 0.093Mpa;

[0043] 4) Take the concentrated paste in step 3) and add it to 2.5 times the mass of 3.0 mol / L hydrochloric acid solution for hydrolysis at 104°C. After hydrolysis, use NaOH to neutralize, wash with water, and dry the filter residue;

[0044] 5) Wrap the filter residue with filter paper and put it into a Soxhlet extractor, add petroleum ether according to the mass ratio of filter residue:petroleum ether of 1:100,...

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Abstract

The invention discloses an alcohol-free extraction method for dioscin. The solubilization effect of a surfactant OP-10 is utilized; water is taken as an extractant, so the cost is low; the pollution is avoided in the extraction process; the dioscin is extracted from Dioscorea zingiberensis Wright; the coating effect of the surfactant OP-10 on the dioscin is damaged when the dioscin is hydrolyzed to form diosgenin by acid; and a hydrolysate of the OP-10 is separated from the diosgenin through a selective extractant, namely gasoline or petroleum ether. The concentration of the OP-10 is 1.5 percent, the OP-10 is sold at 19,000yuan / ton, 7.5 tons of OP-10 is required for extracting 1 ton of dioscin, and the cost is 142.5 thousand yuan and is 40 percent of the cost of an ethanol extraction method, so the extraction cost for the dioscin is low. After the dioscin is extracted from the Dioscorea zingiberensis Wright, the inhibition effect of the dioscin on saccharomycetes is relieved; fermented mash with the alcoholic strength of 10.5 percent can be obtained through fermentation; industrial alcohol can be obtained through distillation; and after fermentation, the content of proteins is improved, so the Dioscorea zingiberensis Wright can be taken as a feed.

Description

technical field [0001] The invention relates to an alcohol-free extraction method of dioscin. Background technique [0002] Diosgenin is a pharmaceutical intermediate with a wide range of uses. It is the basic raw material for the synthesis of protein anabolic hormones, sex hormones, and adrenaline. It is known as the second discovery of the pharmaceutical industry in the 21st century. Dioscorea scutellaria contains 2%-3% dioscin, and dioscin is hydrolyzed into diosgenin. Since the discovery of the medical value of diosgenin in the 1930s, the production of diosgenin has become the focus of research. Formed a separation method (direct acid hydrolysis process) represented by Marker and Wall as the first extraction followed by hydrolysis and Rothrok proposed the separation method of first hydrolysis and then extraction. [0003] Rothrok's direct acid hydrolysis process is considered to be a general method for extracting diosgenin, and its advantages are: simple process, low te...

Claims

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Application Information

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IPC IPC(8): C07J71/00
Inventor 李祥马建中王勇张青赵倩王兰房媛文星
Owner SHAANXI UNIV OF SCI & TECH
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