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The preparation method of echinulin

A technology of Daqu and methanol, applied in the field of chemical analysis, can solve the problems of complex preparation process and difficult to obtain raw materials, achieve high separation efficiency, facilitate solvent recovery, and avoid high-temperature damage

Active Publication Date: 2020-09-29
WULIANGYE +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide the preparation method of Echinulin, to solve the existing Echinulin preparation method raw material is difficult to obtain, the problems such as preparation process complexity

Method used

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  • The preparation method of echinulin
  • The preparation method of echinulin
  • The preparation method of echinulin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] Embodiment 1 adopts the inventive method to prepare Echinulin

[0072] (1) Take Luzhou-flavor pure wheat medium-warm koji (prepared entirely from wheat, control the product temperature of the koji to 35-60°C) 10kg, pulverize, add 20kg of methanol, extract twice at 20°C, each time for 15 days, The extract was filtered and concentrated under reduced pressure to obtain the crude extract of Daqu. Add 10L of distilled water to the crude extract of Daqu, disperse evenly at 60°C, add 10L of petroleum ether to the separatory funnel for extraction three times, collect the petroleum ether phase, and concentrate under reduced pressure to obtain 120g of Daqu extract.

[0073] (2) Stir Daqu extract and 100 mesh normal phase silica gel evenly at a weight ratio of 1:1, perform normal phase column chromatography on silica gel, use petroleum ether / ethyl acetate as the eluting reagent, and use 20:1, 10:1 , 5:1, 2:1, 1:1 (petroleum ether / ethyl acetate, v / v) ratio for gradient elution, 4 ...

Embodiment 2

[0077] Embodiment 2 adopts the inventive method to prepare Echinulin

[0078] (1) Take Luzhou-flavor pure wheat medium-warm koji (prepared entirely from wheat, control the product temperature of the koji to 35-60°C) 10kg, pulverize, add 30kg of ethyl acetate, extract 3 times at 30°C, each time 5 Day, the extract was filtered and concentrated under reduced pressure to obtain 220 g of Daqu extract.

[0079] (2) Evenly stir Daqu extract and 300 mesh normal phase silica gel at a weight ratio of 1:1, perform normal phase column chromatography on silica gel, use petroleum ether / acetone as the eluting reagent, and use 20:1, 10:1, 5 :1, 2:1, 1:1 (petroleum ether / acetone, v / v) ratio for gradient elution, each ratio of elution 6 liters; TLC analysis (petroleum ether / acetone, 3:1, v / v), the parts containing the sample with Rf value of 0.25 were combined and then dried under reduced pressure to obtain component A4.

[0080] (3) Component A4 obtained in the above step (2) is further subj...

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Abstract

The invention relates to a preparation method of Echinulin and belongs to the technical field of chemical analysis. The invention aims to solve the problems in the existing preparation method of the Echinulin that the raw materials are difficult to obtain and the preparation process is complex. The technical scheme for solving the problem is to provide the preparation method of the Echinulin. TheEchinulin is separated from yeast for making hard liquor. The preparation method of the Echinulin comprises the following steps: a, taking the yeast for making hard liquor, crushing, extracting by anorganic solvent and concentrating to obtain the yeast extractum; b, performing silica gel normal phase column chromatography on the yeast extractum, collecting eluent containing the Echinulin and concentrating to obtain a crude product; and c, performing glucan gel column chromatography on the crude product, collecting the eluent containing the Echinulin and concentrating to obtain the Echinulin.Multiple chromatographic techniques are combined, the Echinulin is separated from the yeast for making hard liquor, and the product purity is high.

Description

technical field [0001] The invention relates to a preparation method of Echinulin, which belongs to the technical field of chemical analysis. Background technique [0002] Echinulin, namely 3S,6S,3-[[2-(1,1-Dimethyl-2-propene)-5,7-bis(3,3-Dimethylpropenyl)-1H-indole-3 -yl]methyl]-6-methyl-2,5-piperazinedione, CAS NO: 1859-87-6, molecular weight: 461.64, is a cyclic dipeptide compound, its chemical structure is as follows: [0003] [0004] Previous studies have shown that Echinulin has a wide range of physiological activities, such as anti-virus, anti-tuberculosis, anti-oxidation, anti-inflammation, enhancing immunity, lowering blood pressure and so on. At present, this compound is mainly obtained from single strains, such as Aspergillus chevalieri, Eurotium cristatum, Aspergillus veriecolor, etc., through pure strain culture and isolated from fermentation products. There are many disadvantages, such as many purification procedures, and the difficulty of separation and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D403/06
CPCC07D403/06
Inventor 周韩玲李国友廖勤俭吴林蔚赵东安明哲乔宗伟李杨华王小琴郭艳宋廷富
Owner WULIANGYE
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