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Method for preparing diosgenin through microwave-assisted acidic ionic liquid catalysis

An acidic ionic liquid, diosgenin technology, applied in organic chemistry, steroids, etc., can solve the problems of large discharge, time-consuming biotransformation and enzymatic methods, complicated production processes, etc. Stable, shortened response time effect

Inactive Publication Date: 2016-01-27
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a new method for preparing diosgenin by microwave-assisted acidic ionic liquid catalysis, which solves the problem of discharging a large amount of high-acidity and chlorine-containing sewage, and overcomes the time-consuming and complicated production process of biotransformation and enzymatic methods. question

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Take 100 g of dry powder of Dioscorea Zingiberensis C.H.Wright, add 50% ethanol by volume according to the ratio of solid to liquid (1:10 (g / mL)) and reflux extract for 3 times, each time for 1 hour. After extraction, centrifuge and take the supernatant. The supernatants were combined, and the ethanol was recovered to obtain a saponin-containing aqueous solution. After the aqueous solution was extracted twice with saturated n-butanol at a ratio of 1:1 (V:V), the n-butanol fractions were combined. Recover n-butanol under reduced pressure to dryness to obtain total saponins. Dilute the acidic ionic liquid with deionized water to prepare a 2mol / L ionic liquid solution. According to the ratio of solid to liquid 1:10 (g / mL), it is mixed with saponin and added to the microwave reaction tank. The reaction temperature was set at 80° C., and after reacting under microwave for 20 min, the reaction solution was cooled to room temperature and filtered. The filtrate was rotary e...

Embodiment 2

[0015] Take 200 g of dry powder of Dioscorea Zingiberensis C.H.Wright, add 70% ethanol by volume according to the ratio of solid to liquid (1:15 (g / mL)) and reflux extract twice, each time for 2 hours. After extraction, centrifuge and take the supernatant. The supernatants were combined, and the ethanol was recovered to obtain a saponin-containing aqueous solution. After the aqueous solution was extracted twice with saturated n-butanol at a ratio of 1:1 (V:V), the n-butanol fractions were combined. Recover n-butanol under reduced pressure to dryness to obtain total saponins. Dilute the acidic ionic liquid with deionized water to prepare a 4mol / L ionic liquid solution. According to the ratio of solid to liquid 1:10 (g / mL), it is mixed with saponin and added to the microwave reaction tank. The reaction temperature was set at 100° C., and after reacting under microwave for 15 minutes, the reaction liquid was cooled to room temperature and filtered. The filtrate was rotary eva...

Embodiment 3

[0017] Take 300 g of dry powder of Dioscorea Zingiberensis C.H.Wright, add 80% ethanol at a volume ratio according to the ratio of solid to liquid (1:20 (g / mL)) and reflux extract twice, each time for 1 hour. After extraction, centrifuge and take the supernatant. The supernatants were combined, and the ethanol was recovered to obtain a saponin-containing aqueous solution. After the aqueous solution was extracted twice with saturated n-butanol at a ratio of 1:1 (V:V), the n-butanol fractions were combined. Recover n-butanol under reduced pressure to dryness to obtain total saponins. Dilute the acidic ionic liquid with deionized water to prepare a 6mol / L ionic liquid solution. According to the ratio of solid to liquid 1:20 (g / mL), it is mixed with saponin and added to the microwave reaction tank. The reaction temperature was set at 110° C., and after reacting under microwave for 10 min, the reaction solution was cooled to room temperature and filtered. The filtrate was rotar...

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Abstract

The present invention relates to a new method for preparing diosgenin through microwave-assisted acidic ionic liquid catalysis, and belongs to the technical field of agricultural product deep processing and medicine. The method comprises: extracting the total saponin in the rhizome of dioscorea zingiberensis or other dioscoreaceae plants with an ethanol aqueous solution, carrying out catalytic hydrolysis on the saponin in a microwave reaction tank through the co-action of microwaves and an acidic ionic liquid to obtain diosgenin, cooling the reaction liquid, filtering, drying the filtration residue, extracting the diosgenin with petroleum ether, and removing water from the filtrate to obtain the ionic liquid, wherein the recovered ionic liquid can be recycled. According to the present invention, the acidic ionic liquid is used to replace the inorganic acid in the traditional hydrolysis method, such that the problem that a large amount of high-acidity chlorine-containing sewage is discharged is solved; the problems of long time consumption and complex production process of the biological conversion method and the enzyme method are overcome; with the microwave-assisted technology, the reaction time can be significantly shortened; the ionic liquid can be recycled so as to reduce the production cost; and the method is the efficient and green environmental protection diosgenin preparation method.

Description

technical field [0001] The invention relates to a method for preparing diosgenin by microwave-assisted acidic ionic liquid catalysis. Specifically, saponins extracted from the dried rhizomes of Dioscoreaceae plants are used as raw materials to generate diosgenin through microwave-assisted catalysis in an acidic ionic liquid system . It belongs to the field of deep processing of agricultural products and medical technology. Background technique [0002] Dioscorea Zingiberensis C.H.Wright is an important medicinal plant rich in diosgenin. Diosgenin is a basic raw material and starting intermediate for the synthesis of hormone drugs, and almost all steroid hormone drugs can be synthesized based on it. In the drug family, steroid hormone drugs are the second largest class of drugs after antibiotics. my country has used diosgenin to synthesize more than 100 kinds of drugs. In addition to hormones, anti-inflammatory, hypolipidemic, anti-viral, anti-allergic, contraceptive and o...

Claims

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Application Information

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IPC IPC(8): C07J71/00
Inventor 王洪新汪朋马朝阳娄在祥吕文平
Owner JIANGNAN UNIV
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