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Method for producing tilmicosin and tilmicosin phosphate by utilizing tylosin fermentation broth

A technology of tilmicosin phosphate and tylosin, which is applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of unsuitability for large-scale industrial production, difficulty in ensuring product quality, and high safety requirements. Achieve the effect of short and efficient production process route, reduce solvent consumption, and reduce three waste discharge

Inactive Publication Date: 2018-11-23
CHINA ANIMAL HUSBANDRY IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The feature of this process is that although the process route is shorter than the typical production process, it still needs to go through two solvent extractions, resulting in large solvent loss and relatively long steps; and finally, the tilmicosin is obtained by vacuum drying the solvent extract, which is very difficult. High safety requirements lead to high production costs and are not suitable for large-scale industrial production; moreover, this process mainly uses phase transfer to purify the product, and finally obtains the product by completely evaporating the solvent. Precursor substances and reaction by-products will completely remain in the final product with the removal of the solvent, and the product quality is not easy to guarantee

Method used

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  • Method for producing tilmicosin and tilmicosin phosphate by utilizing tylosin fermentation broth
  • Method for producing tilmicosin and tilmicosin phosphate by utilizing tylosin fermentation broth
  • Method for producing tilmicosin and tilmicosin phosphate by utilizing tylosin fermentation broth

Examples

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Effect test

Embodiment 1

[0061] Tylosin fermentation liquid obtained by fermentation method 100m 3 , the titer of tylosin is 15600u / ml, add concentrated sulfuric acid while stirring, adjust the pH value of the fermentation broth to 2.5, then raise the temperature to 65-75°C, keep it warm for 1 hour, and determine tylosin A by high performance liquid chromatography The residual content is 1.21%, and the area ratio of Tylosin B reaches 98.79%. Add filter aid diatomaceous earth 0.5% (W / V) then in fermented liquid; Continue to stir 0.5 hour; Filter through plate frame and pass into a certain amount of water washing filter cake to obtain Tylosin B filtrate 125m 3 , The titer is 11826u / ml.

[0062] Add Tylosin B filtrate to about 40m 3 Butyl acetate, while stirring, add 20% sodium hydroxide solution, control the pH value of the aqueous phase at 11-12, operate the stirring speed at 15 rpm during the pH adjustment process, and continue stirring for 0.5 hours after the pH reaches the control range; stop stir...

Embodiment 2

[0065] Tylosin fermentation liquid obtained by fermentation method 102m 3 , the titer of tylosin is 13600u / ml, add concentrated sulfuric acid while stirring, adjust the pH value of the fermentation broth to 2.5, then raise the temperature to 65-75°C, keep it warm for 1 hour, and measure the residue of tylosin A by high performance liquid chromatography 1.25%, the area ratio of Tylosin B reached 98.75%. Then add the filter aid perlite 0.5% (W / V) in the fermented liquid; Continue to stir for 0.5 hour; Filter through the plate frame and feed a certain amount of water to wash the filter cake to obtain the tylosin B filtrate 129m 3 , The titer is 10216u / ml.

[0066] Add Tylosin B filtrate to about 40m 3 Butyl acetate, while stirring, add 20% sodium hydroxide solution, control the pH value of the aqueous phase at 11-12, operate the stirring speed at 15 rpm during the pH adjustment process, and continue stirring for 0.5 hours after the pH reaches the control range; stop stirring, ...

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Abstract

The invention belongs to the field of pharmacy and particularly discloses a method for producing tilmicosin and tilmicosin phosphate by utilizing a tylosin fermentation broth. The method comprises thefollowing steps of performing hydrolysis pretreatment and filtering on the tylosin fermentation broth to obtain a tylosin B filtrate, then performing extraction separation on the tylosin B filtrate,performing catalyzed synthesis to obtain the tilmicosin, performing water-phase extraction, decoloration, crystallization and solid-liquid separation to obtain a wet tilmicosin solid, and drying the wet tilmicosin solid to obtain a tilmicosin product, or dissolving the wet tilmicosin solid with strong phosphoric acid to prepare a tilmicosin phosphate product. In the method, by directly taking thetylosin fermentation broth as a starting material to extract and synthesize the tilmicosin product or the tilmicosin phosphate product, the production technology is simplified, the production time isremarkably shortened, the production efficiency is improved, the yield of the product is increased, the quality of the product is improved, the production cost is lowered, loss of an organic solvent is reduced, emission of the three wastes is remarkably reduced, and the method has the advantages of energy conservation, consumption reduction, safe environment, excellent quality, cost reduction andthe like.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular relates to a method for producing tilmicosin and tilmicosin phosphate by using tylosin fermentation broth. Background technique [0002] Tilmicosin is an over-the-counter drug. It is a semi-synthetic macrolide antibiotic for livestock and poultry developed in the 1980s. It is a semi-synthesized antibiotic for livestock and poultry from a hydrolyzate of tylosin. The medicinal form is Its phosphate or alkali has a molecular weight of 869.15. Tilmicosin is a product obtained by the amination reaction of aldehyde groups after desugaring tylosin. The amination reaction adopts a catalytic synthesis reaction using formic acid as a catalyst. Its antibacterial effect is similar to that of tylosin, mainly against gram-positive bacteria, and also effective against a small number of gram-negative bacteria and mycoplasma. Rhodomycin is strong. Rapid absorption after oral administration or subcutan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/00C07H1/06
CPCC07H1/00C07H1/06C07H17/08
Inventor 梁景乐靳连标李子勇牛志强张正海
Owner CHINA ANIMAL HUSBANDRY IND
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