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Method for pressurized ethanol/water extraction of diosgenin

A technology for extracting diosgenin and water, which is applied in the production of steroids, organic chemistry, bulk chemicals, etc., can solve the problems of polluting the environment, large amount of acid, etc., achieve less impurity content, reduce emissions, and avoid acid pollution Effect

Inactive Publication Date: 2018-09-25
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method uses an acidic ionic liquid instead of a commonly used inorganic acid to solve the problems of excessive acid consumption and serious environmental pollution in the process of preparing diosgenin in modern industry; replaces pure water with an ethanol / water mixed solvent to avoid the large amount of diosgenin contained in diosgenin. The impact of molecular substances on the extraction process; the use of macroporous resins for separation and purification instead of gasoline or petroleum ether extraction solves the problem of using flammable and explosive solvents. The most important thing is that both acidic ionic liquids and macroporous resins can be recycled and reused

Method used

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  • Method for pressurized ethanol/water extraction of diosgenin
  • Method for pressurized ethanol/water extraction of diosgenin

Examples

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Effect test

Embodiment 1

[0018] A method for extracting diosgenin with pressurized ethanol / water, which is carried out according to the following steps: (1) take dried rhizomes of pangolin or other Dioscoreaceae plants, and grind them through a 24-60 mesh sieve according to a conventional method. (2) According to the solid-liquid ratio of 1: 10 (g / mL) ratio, adding volume ratio is 50% ethanol, then adding acidic ionic liquid, finally making the pH of the solvent in the extraction tank be 2, then at the extraction temperature of 100 ° C, the extraction pressure Extract for 25min under the condition of 0.2MPa. (3) After the extraction, let the extract cool to 50-60°C, filter, put the filtrate on a macroporous resin column, first elute the acidic ionic liquid with water, then gradually increase the ethanol concentration, elute diosgenin, and concentrate the eluent , after drying or crystallization, diosgenin can be obtained.

Embodiment 2

[0020] A method for extracting diosgenin with pressurized ethanol / water, which is carried out according to the following steps: (1) take dried rhizomes of pangolin or other Dioscoreaceae plants, and grind them through a 24-60 mesh sieve according to a conventional method. (2) According to the solid-liquid ratio of 1: 15 (g / mL), it is 60% ethanol to add the volume ratio, then add the acidic ionic liquid, finally make the pH of the solvent in the extraction tank be 3, then at the extraction temperature of 125 ° C, the extraction pressure It is extracted for 45min under the condition of 0.3MPa. (3) After the extraction, let the extract cool to 50-60°C, filter, put the filtrate on a macroporous resin column, first elute the acidic ionic liquid with water, then gradually increase the ethanol concentration, elute diosgenin, and concentrate the eluent , after drying or crystallization, diosgenin can be obtained.

Embodiment 3

[0022] A method for extracting diosgenin with pressurized ethanol / water, which is carried out according to the following steps: (1) take dried rhizomes of pangolin or other Dioscoreaceae plants, and grind them through a 24-60 mesh sieve according to a conventional method. (2) According to the solid-liquid ratio of 1:20 (g / mL), it is 80% ethanol to add the volume ratio, then add the acidic ionic liquid, finally make the pH of the solvent in the extraction tank be 4, then at the extraction temperature of 150 ° C, the extraction pressure Extract for 25min under the condition of 0.5MPa. (3) After the extraction, let the extract cool to 50-60°C, filter, put the filtrate on a macroporous resin column, first elute the acidic ionic liquid with water, then gradually increase the ethanol concentration, elute diosgenin, and concentrate the eluent , after drying or crystallization, diosgenin can be obtained.

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Abstract

The invention discloses a method for extracting and preparing diosgenin from Dioscorea nipponica Makino or other Dioscoreaceae plants, belonging to the technical fields of deep processing of agricultural products and medicine. The method comprises the following steps: pulverizing Dioscorea nipponica Makino or other Dioscoreaceae plants according to a conventional method, adding the pulverized plants into a pressurized extraction tank, then adding a proper amount of ethanol / water as a solvent, adding acidic ionic liquid as a catalyst, carrying out extraction at a certain pressure and a certaintemperature for a certain period of time, cooling extract room temperature after extraction, carrying out filtering to remove herbal residues, appropriately concentrating a filtrate, allowing concentrated liquid to passed through a macroporous resin column, carrying out washing with water to remove acidic ionic liquid, then carrying out elution by using ethanol with an appropriate concentration, and subjecting eluate to concentration and drying so as to obtain diosgenin. According to the method, the acidic ionic liquid is used for replacing commonly used inorganic acid, so the problems of excessive acid consumption and serious pollution environment in modern industrial preparation of diosgenin are overcome; at the same time, elution with the macroporous resin column is used for replacing gasoline or petroleum ether extraction, so the problem of usage of flammable and explosive solvents is overcome; and the acidic ionic liquid and macroporous resin can be recycled. The method has the characteristics of safety, conservation of cost and environmental protection.

Description

technical field [0001] The invention belongs to the technical field of deep processing of agricultural products and medicine, and discloses a method for extracting and preparing diosgenin from pangolin or other Dioscoreaceae plants. Background technique [0002] The water-soluble saponins contained in Pangolinus and other Dioscoreaceae plants become diosgenin after hydrolysis, and diosgenin is an ideal basic raw material and intermediate for the synthesis of steroid hormone drugs, such as corticosteroids and steroidal contraceptives. At present, nearly 300 steroid hormone drugs can be synthesized from diosgenin, and steroid hormone drugs are the second most consumed drugs in the world, which determines that diosgenin has extremely high economic value. At present, the traditional pre-fermentation-acid hydrolysis method is mostly used in domestic extraction of diosgenin, but this method has long reaction time, high water consumption, serious pollution, and low utilization rate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J71/00
CPCC07J71/0005Y02P20/54
Inventor 赵文英朱庆书徐艳丽杨玉莹孙彦妮王倩
Owner QINGDAO UNIV OF SCI & TECH
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