Preparation method of pure nosiheptide

A technology of nosiheptide and pure product, applied in the field of preparation of pure nosiheptide, can solve the problems of long production cycle, increased workload, limited application scope, etc., and achieves simple production process, high product purity, and high production efficiency. Effect

Inactive Publication Date: 2016-03-23
山东胜利生物工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The second method also needs to adjust the pH value of the system during the whole process, which increases a certain amount of work. Moreover, after nosiheptide is precipitated with an acidic aqueous solution, the amount of organic solvent used cannot be reused, and the discarded solution will also environmental issues
The third method is to directly use the fermentation broth to extract nosiheptide, so the scope of application of the method is limited, and the whole extraction process has cumbersome steps and a long production cycle, which is not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 1000 g of nosiheptide flash powder, add 1000 mL of water and 3000 mL of N,N-dimethylformamide, stir at a constant speed for 1 hour with a mechanical stirring speed of 50 rpm, and control the temperature of the entire system at 25 °C; After the solid-liquid separation of the system, the solid bacterial residue was used for later use. The leaching solution was placed in a rotary evaporator, and 2000 mL of N,N-dimethylformamide was distilled off in a 70°C water bath, and the organic solvent was recovered to obtain 1880 mL of concentrated solution. . Add 2000 mL of water and 2000 mL of petroleum ether to the concentrated solution, stir at 100 rpm for 3 hours at 25 °C, and after suction filtration, the filter cake is transferred to a vacuum drying box, and dried at 60 °C under vacuum degree -0.09MPa for 16 hours. 49.7 g of nosiheptide with a content of 85.4% was obtained. The pure nosiheptide prepared by the invention can be made into premixes of various specification...

Embodiment 2

[0035]Weigh 1000 g of nosiheptide flash powder, add 2500 mL of water and 2500 mL of tetrahydrofuran, stir at a constant speed with mechanical stirring at a speed of 150 r / min, stir for 2 hours, and control the temperature of the entire system at 35 °C; Afterwards, the solid bacterial residue was used for later use, and the leaching solution was placed in a rotary evaporator, and 2000 mL of tetrahydrofuran was evaporated in a 40° C. water bath, and the solvent was recovered to obtain 2850 mL of a concentrated solution. Add 3000 mL of water and 3000 mL of methyl tert-butyl ether to the concentrated solution, stir at 100 rpm for 3 hours at 35°C, and after suction filtration, the filter cake is transferred to a vacuum drying box, and dried at 60°C under vacuum degree-0.09MPa for 10 hours. 46.3 g of nosiheptide with a content of 92.5% was obtained after pulverization. The pure nosiheptide prepared by the invention can be made into premixes of various specifications or further purif...

Embodiment 3

[0037] Weigh 1000g of nosiheptide flash powder, add 1000mL of water and 4000mL of tetrahydrofuran, stir at a constant speed with mechanical stirring at a speed of 100 rev / min, stir for 3 hours, and control the temperature of the entire system at 25 °C; After that, the solid bacterial residue was used for later use, and the leaching solution was placed in a rotary evaporator, and 3000 mL of tetrahydrofuran was evaporated in a 40° C. water bath, and the solvent was recovered to obtain 2410 mL of a concentrated solution. Add 3000 mL of water and 3000 mL of n-hexane to the concentrated solution, stir at 100 rpm for 3 hours at 25°C, and after suction filtration, the filter cake is transferred to a vacuum drying box, dried at 60°C under vacuum of -0.09MPa for 10 hours, and pulverized. 51.2 g of nosiheptide with a content of about 96.0% was obtained. The pure nosiheptide prepared by the invention can be made into premixes of various specifications or further purified to make nosihept...

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PUM

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Abstract

The invention relates to a preparation method of pure nosiheptide. The method comprises the steps that nosiheptide flashing powder is used as raw materials, a solvent is added for digestion, the temperature is controlled within 20-60 DEG C, and stirring is performed at the uniform rotating speed of 50-300 r / min for 1-3 h; a leaching solution obtained after the raw materials are processed is separated from solid mushroom dregs, the leaching solution is concentrated on a rotary evaporator at the temperature of 30-70 DEG C, and the organic solvent is recycled to obtain a concentrated solution; water and an elution agent are added into the concentrated solution, stirring is performed at the rotating speed of 100-400 r / min for 1-5 h, and then suction filtration is performed to obtain filter cakes; the filter cakes are placed into a vacuum drying oven, drying is performed at the temperature of 20-70 DEG C and the vacuum degree of minus 0.09 MPa for 6-16 h, and smashing is performed to obtain the pure nosiheptide. The method has the advantages that the production technology is simple, operation is convenient, the production efficiency is high, the product purity is high, and economy and environmental protection are achieved; the extracted nosiheptide can be prepared to obtain nosiheptide raw drugs or nosiheptide premixing agents of different specifications.

Description

technical field [0001] The invention relates to a preparation method of pure nosiheptide, belonging to the field of chemical pharmacy. Background technique [0002] Nosiheptide is a sulfur-containing polypeptide antibiotic, which is not easily absorbed in the intestinal tract and can be quickly decomposed when excreted, so it has no residue, is not easy to develop drug resistance, and has no cross-resistance with other antibiotics, and has little impact on the environment. Features. Nosiheptide is an environmentally friendly feed additive. [0003] In 1961, French scientists discovered nosiheptide in the fermentation broth of Streptomycesactuosus40037, which was then trial-produced by the Rhone-Planck Company and conducted animal feeding experiments in Belgium, France, the United States and other countries and regions, and found that it is an excellent effect. However, due to its low yield and high cost, it has not been widely promoted. [0004] In 1970, Japan's Mitsubish...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P21/02C07K5/078C07K1/36C07K1/34C07K1/30
CPCC07K5/06139C12P21/02
Inventor 赵学鹏邱向东赵才兵刘正光闵江陈宁张铜镇
Owner 山东胜利生物工程有限公司
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