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Method for preparing natural 4-hydroxy-isoleucine

A technology of isoleucine and hydroxyl, which is applied in the field of preparation of natural 4-hydroxy-isoleucine, can solve the problems of high cost, difficult synthesis, complex processing technology, etc., and achieve the effect of low cost

Inactive Publication Date: 2013-04-10
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

4-Hydroxy-isoleucine is difficult to synthesize due to its three chiral carbon atoms
So far, domestic and foreign patent documents have reported the method of extracting 4-hydroxy-isoleucine from fenugreek seeds, the content of which is 10-70%. Publication number: CN 1397545A; US2004 / 0009247 A1; Publication number: CN 1955160A , but its processing technology is complicated, the cost is high, and it has certain pollution to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take 10 kg of fenugreek seeds, pulverize them, add 60 kg of 30% ethanol aqueous solution, extract 3 times at 60°C for 2 hours each time, filter, and combine the filtrates; concentrate the filtrate until the ethanol is removed, and then centrifuge to remove the precipitate to obtain a solution The solution is adsorbed with conventional macroporous adsorption resin D-101, washed with 3 times of water, and the water eluate containing target components is collected, and the macroporous adsorption resin can be reused after cleaning with ethanol; the water eluate After concentrating to 1 / 4 of the original volume, according to the mass ratio of concentrate: silica gel = 1:2, mix in 100-200 mesh silica gel, and carry out conventional stirring and drying; use the mixed solution of ethyl acetate, ethanol and water as the mobile phase Carry out silica gel column chromatography, wherein ethyl acetate: ethanol: the volume ratio of water is 3: 2: 1, elute afterwards, collect the eluen...

Embodiment 2

[0021] Take 10 kg of fenugreek seeds, pulverize them, add 30 kg of 5% ethanol aqueous solution, extract twice at 90°C for 3 hours each time, filter, and combine the filtrates; concentrate the filtrate, remove ethanol and then centrifuge to remove the precipitate to obtain a solution; The solution is adsorbed with conventional macroporous adsorption resin AB-8, washed twice with water, and the water eluate containing the target component is collected. The macroporous adsorption resin can be reused after being washed with ethanol; the water eluate is concentrated to 1% of the original volume. / 4, according to the mass ratio of concentrate: silica gel=1:2, mix 100-200 mesh silica gel, carry out conventional stirring and drying; Carry out silica gel column chromatography with the mixed solution of ethyl acetate, ethanol and water as mobile phase, wherein acetic acid The volume ratio of the mixed solution of ethyl ester, ethanol and water is: ethyl acetate: ethanol: water = 9: 5: 0,...

Embodiment 3

[0023] Take 10 kg of fenugreek seeds, crush them, add 100 kg of 95% ethanol aqueous solution, extract twice at 30°C for 2 hours each time, filter, and combine the filtrates; concentrate the filtrate, remove ethanol and then centrifuge to remove the precipitate to obtain a solution; Adsorb with conventional macroporous adsorption resin DM-1300, wash with water 3 times, collect the water eluate containing the target components, the macroporous adsorption resin can be reused after washing with ethanol; concentrate the water eluate to 1 / 1 of the original volume 4. According to the mass ratio of concentrated liquid: silica gel = 1:2, mix 100-200 mesh silica gel for conventional stirring and drying; use a mixed solution of ethyl acetate, ethanol and water as the mobile phase for silica gel column chromatography, wherein ethyl acetate , the volume ratio of the mixed solution of ethanol and water is ethyl acetate: ethanol: water=5: 3: 1, after elution, collect the eluent containing tar...

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Abstract

The invention discloses a method for preparing natural 4-hydroxy-isoleucine, which belongs to the field of pharmacy. The method comprises the following steps: crushing fenugreek seeds and then extracting the powder with ethanol; adsorbing the extracting solution with macroporous adsorption resin column after recovering the ethanol, eluting the extracting solution with water, adding silica gel into the extracting solution after concentration, and mixing the mixture evenly; drying the mixture, and performing silica gel column chromatography by using mixed solution of ethyl acetate, ethanol and water as a mobile phase; collecting the eluent containing target components, recovering the solvent, and drying the eluent to obtain a crude product of the 4-hydroxy-isoleucine; dissolving the crude product in an organic solvent by heating until the mixture is saturated; and filtering the mixture, and placing the mixture in low temperature environment for crystallization so as to obtain a pure product of the 4-hydroxy-isoleucine. The method does not need acid, alkali or chloroform and other toxic chemical reagents, the preparation process is environmentally-friendly, and the cost is low, thus the method is suitable for industrial scale production.

Description

technical field [0001] The invention relates to a preparation method of natural 4-hydroxy-isoleucine, which belongs to the technical field of medicine production. Background technique [0002] At present, the number of deaths caused by complications of diabetes has ranked third after cardiovascular diseases and cancers, which has attracted great attention from all countries. Traditional Chinese medicine has a long history of treating diabetes, and it has been found that preparing active ingredients with high efficiency and low toxicity is an important way for new drug development. Fenugreek (Trigonella foenum graecum L.) is a plant of the Papilionaceae subfamily of Fabaceae. Its seeds are well-known traditional Chinese medicine for tonifying yang. It has a long history of medicinal and edible use at home and abroad. Its nutrition and safety have also been investigated. Research (Nutrition Research, 1996, 16:1495). In recent years, the research results at home and abroad sh...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/22C07C227/40A61P3/10
Inventor 曹建新樊建赵天瑞刘会灵程桂广
Owner KUNMING UNIV OF SCI & TECH
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