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Separation method of high-purity diosgenin

A technology of diosgenin and separation method, applied in the directions of steroids, organic chemistry, etc., can solve problems such as difficulty in separation and purification of dioscin, achieve good flocculation effect, reduce pollution, and ensure the effect of clean production

Active Publication Date: 2014-08-06
BAIHE YONGHONG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to overcome the defects in the above-mentioned prior art, the object of the present invention is to provide a method for separating high-purity diosgenin, which is simple to operate and environmentally friendly, and can effectively solve the problem of difficult separation and purification of diosgenin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A flocculation extraction method for diosgenin, comprising rough separation and fine treatment steps:

[0040] Coarse separation:

[0041] 1) First, take 100g of Dioscorea scutellaria with a particle size of 80 mesh, and add 1000mL of it to a concentration of 25.8×10 -3 mol / L sodium lauryl sulfate solution, soaked at room temperature for 2 hours, then ultrasonically extracted at an ultrasonic frequency of 25.8KHz for 30 minutes, and centrifuged to obtain Dioscorea saponin extract 1 and Dioscorea scutellaria filter residue; Filter residue: sodium lauryl sulfate = 1g: 8mL solid-liquid ratio. Add the filter residue of Dioscorea scutellaria to lauryl sulfuric acid solution. Under the same ultrasonic conditions, perform ultrasonic extraction and centrifugation to obtain extract 2 and filter residue; Then according to the solid-liquid ratio of filter residue: sodium lauryl sulfate = 1g: 5mL, add the filter residue into sodium lauryl sulfate, ultrasonically extract under the ...

Embodiment 2

[0050] A flocculation extraction method of diosgenin, comprising the following steps:

[0051] Coarse separation:

[0052] 1) First, take 100g of Dioscorea scutellaria with a particle size of 80 mesh, and add 800mL of it to a concentration of 25.8×10 -3 mol / L sodium lauryl sulfate solution, soaked at room temperature for 3 hours, ultrasonically extracted at an ultrasonic frequency of 25.8KHz for 30 minutes, and centrifuged to obtain Dioscorea saponin extract 1 and Dioscorea scutellaria filter residue; Filter residue: sodium lauryl sulfate = 1g: 10mL solid-liquid ratio. Add the filter residue of Dioscorea scutellaria to lauryl sulfuric acid solution. Under the same ultrasonic conditions, perform ultrasonic extraction and centrifugation to obtain extract 2 and filter residue; Then add the filter residue into sodium lauryl sulfate according to the solid-liquid ratio of filter residue: sodium lauryl sulfate = 1g: 7mL, ultrasonically extract under the same conditions, and then cen...

Embodiment 3

[0061] A flocculation extraction method of diosgenin, comprising the following steps:

[0062] Coarse separation:

[0063] 1) First, take 100g of Dioscorea scutellaria with a particle size of 100 mesh, and add 900mL of it to a concentration of 25.8×10 -3 mol / L sodium lauryl sulfate solution, soaked at room temperature for 4 hours, ultrasonically extracted at an ultrasonic frequency of 25.8KHz for 30 minutes, and centrifuged to obtain Dioscorea saponin extract 1 and Dioscorea scutellaria filter residue; : Sodium lauryl sulfate=1g: 9mL solid-liquid ratio Dioscorea scutellaria filter residue is added in lauryl sulfuric acid solution, under the same ultrasonic condition, ultrasonic extraction, centrifugation, obtain extract 2 and filter residue; Then According to the solid-liquid ratio of filter residue: sodium lauryl sulfate = 1g: 6mL, filter residue was added to sodium lauryl sulfate, ultrasonically extracted under the same conditions, and then centrifuged to collect extract 3,...

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Abstract

The invention discloses a separation method of high-purity diosgenin and belongs to the technical field of pharmaceutical raw material production. The method is characterized by comprising the steps as follows: adopting the ultrasonic assisted sodium lauryl sulfate extraction technology and utilizing the solubilization action of sodium lauryl sulfate to extract dioscin from dioscorea zingiberensis; adopting the flocculation technology to separate the dioscin from the extracting solution to obtain crude dioscin; obtaining crude diosgenin through hydrolyzation, filtration, water scrubbing, drying, reflux extraction and cooling crystallization of the crude dioscin; obtaining precision processed diosgenin through batch splitting precision processing of the crude diosgenin in warm water. The separation method has the benefits that the precision processing of the method overcomes the deficiency of difficulty in diosgenin separation and purification, and the degree of purity of the precision processed diosgenin is above 98.5%.

Description

technical field [0001] The invention belongs to the technical field of production of pharmaceutical raw materials, and in particular relates to a method for separating high-purity diosgenin. Background technique [0002] Around the pollution and cost problems of producing diosgenin, people have done a lot of research work and made some achievements. Before 2003, the pre-fermentation-acid hydrolysis process was widely used in my country to produce diosgenin. Compared with the traditional acid direct hydrolysis process, the yield of diosgenin was improved, but the amount of acid used was basically equivalent to the traditional process. Therefore, The pollution is basically the same as the traditional process. In the course of the research, it was found that the production process of diosgenin used a lot of acid, and the source of the high COD and BOD values ​​in the wastewater was that while the diosgenin in Dioscorea scutellaria was hydrolyzed into diosgenin, the Starch and ...

Claims

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Application Information

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IPC IPC(8): C07J71/00
Inventor 李祥师春兰王丽萍张彬
Owner BAIHE YONGHONG CHEM CO LTD
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