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Method for efficiently preparing deoxynivanol

A falkenol and high-efficiency technology, applied in the field of natural product extraction, can solve the problems of long production cycle, low product purity, waste of manpower and material resources, etc., to save usage and sample processing time, reduce production costs, and improve production. The effect of efficiency

Inactive Publication Date: 2013-11-20
SHANGHAI ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The current preparation methods of vomitoxin include (1) Colvin et al. use chemical synthesis to synthesize deoxynivalenol, but the purity and yield of the synthetic compound are not suitable for industrial production
(2) Altpeter etc. and Ehrlich etc. have developed a kind of preparation method of deoxynivalenol respectively, but these methods need to pass through complex multi-step column chromatography, the production cycle is long, waste a lot of manpower and material resources, and the product obtained not high purity
However, this method needs to wash the chromatographic column repeatedly after each injection, or the sample needs to be separated by the chromatographic column twice, which greatly increases the production cost and production cycle
(4) He et al. developed a high-speed countercurrent liquid chromatography method based on liquid-liquid extraction for the separation and purification of deoxynivalenol. (<8 times) Its chromatographic separation system needs to be updated, which greatly limits its industrial production efficiency

Method used

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  • Method for efficiently preparing deoxynivanol
  • Method for efficiently preparing deoxynivanol
  • Method for efficiently preparing deoxynivanol

Examples

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Embodiment 1

[0029] Example 1: Fusarium was cultured on potato medium at 28°C for 3 days in the dark, and then the mycelia were inoculated into 200 ml of carboxymethyl cellulose medium and vibrated at 200 r / min at 25°C for 1 day to obtain Fusarium graminearum Spore liquid, adjust the concentration to 1.0×10 by hemocytometer counting 5pcs / ml and save for later use. Weigh 50g of rice into a 200m1 Erlenmeyer flask, add 20m1 of deionized water, and sterilize at 121°C for 30 minutes; inoculate the bacteria block or spore liquid into the sterilized rice medium, and place it at 28°C for 10 days; The rice medium was dried in a drying oven at 50°C for 24 hours, and then crushed into a uniform powder using a high-speed pulverizer. Weigh 100g of dry powder and place it in a conical flask and add different extraction solvents (acetonitrile, 84% acetonitrile water, 50% acetonitrile water, methanol, 70% methanol water, 50% methanol water, ethyl acetate, water) to extract, the extract Place at 4°C for ...

Embodiment 2

[0030] Embodiment 2: The preparation of Fusarium graminearum spore liquid is the same as that in Embodiment 1. Weigh 50g of corn into a 200ml Erlenmeyer flask, add 20ml of deionized water, and sterilize at 121°C for 30min; the rest of the steps are the same as in Example 1.

Embodiment 3

[0031] Example 3: The preparation of Fusarium graminearum spore liquid was the same as in Example 1. Weighed 50 g of wheat into a 200 ml Erlenmeyer flask, added 20 ml of deionized water, and sterilized at 121° C. for 30 minutes; the rest of the steps were the same as in Example 1.

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Abstract

The invention aims to provide a method capable of preparing a large number of deoxynivanol, which is simple, quick and low in cost. The method comprises the following steps: inoculating fusarium into a solid culture medium to obtain a culture with high-content deoxynivanol; extracting; preparing a liquid phase; and separating, purifying and recrystallizing to obtain the deoxynivanol compound with high purity. The process is simple to operate and high in preparation speed, and the production cost can be greatly reduced. The purity reaches above 98%. The deoxynivanol can serve as a standard substance applied to safety monitoring of the deoxynivanol of grains and food. The method also fills up the gap of the field of preparation of fungaltoxin standard substances in China.

Description

technical field [0001] The invention belongs to the field of natural product extraction, and in particular relates to a method for extracting, separating and purifying secondary metabolites from a solid medium inoculated with Fusarium fungus. Background technique [0002] Deoxynivalenol (deoxynivalenol, 3,7,15-trihydroxy-12,13-epoxytrichothecene-9-en-8-one), also known as vomitoxin, is produced by Fusarium graminearum, A trichothecene B produced by fungi such as Fusarium oxysporum, Fusarium moniliforme, Fusarium cladosporum, Fusarium pink and Fusarium nivale infecting cereal crops under suitable temperature and humidity conditions Toxoid. It was first isolated in oats by the Japanese Morooka in 1972. DON is resistant to high temperature and high pressure, does not decompose in weak acid, and has very stable chemical properties. At the same time, it is easily soluble in polar solvents such as water, acetonitrile, methanol and ethyl acetate. [0003] Deoxynivalenol is one ...

Claims

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Application Information

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IPC IPC(8): C12P17/18C07D493/10C12R1/77
Inventor 武爱波赵志勇宋素泉王建华刘娜聂冬霞杨宪立
Owner SHANGHAI ACAD OF AGRI SCI
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