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Method for synthesizing tilmicosin and tilmicosin phosphate through using tylosin broth

A technology of tilmicosin phosphate and tylosin, which is applied in chemical instruments and methods, organic chemistry, sugar derivatives, etc., can solve the problems of increased loss of intermediates, cumbersome process routes, and high production costs, and reduce the use of Equipment, simplified production process, and low production cost

Active Publication Date: 2012-09-12
宁夏泰瑞制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The common point of the above-mentioned processes is to use the prepared finished product tylosin salt or alkali to prepare tilmicosin again, resulting in cumbersome process route, long production cycle, increased loss of intermediates, high production cost, and high production cost. Low efficiency, low yield of finished product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Tylosin fermentation broth volume 50m 3 , the potency is 13210u / ml, and the total fermentation value is 660.5. Control the temperature of the fermentation broth at 20-30°C, add 10-20% polyaluminum sulfate solution, adjust the pH of the fermentation broth to 1.2, continue stirring for 10 minutes, and the titer after acidification is 14697u / ml; then adjust the pH of the fermentation broth with 5.4% ammonia water , control the pH at 3.2, stir for 10 minutes, let stand for 50 minutes, and filter the fermentation broth with a plate and frame filter to obtain tylosin filtrate 40m 3 , After alkalization, the titer is 15819u / ml.

[0029] Use organic solvent butyl acetate to extract tylosin solution, the volume of butyl acetate is 16m 3 . During the extraction process, the temperature was controlled at 40-42°C. Carry out secondary countercurrent extraction with a centrifuge, the extraction ends, the raffinate titer is 267u / ml, and the volume of butyl acetate is 15.8m 3 . Add...

Embodiment 2

[0037] Tylosin fermentation broth volume 50m 3 , the potency is 13953u / ml, and the total fermentation value is 697.7. Control the temperature of the fermentation broth at 24-26°C, add 15% polyaluminum sulfate solution, adjust the pH of the fermentation broth to 2.1, continue stirring for 12 minutes, and the titer after acidification is 15813 u / ml; then adjust the pH of the fermentation broth with 13.8% ammonia water, Control the pH at 5.2, stir for 13 minutes, let stand for 55 minutes, and filter the fermentation broth with a plate and frame filter to obtain a tylosin filtrate of 39.2m 3 , After alkalization, the potency is 16980u / ml.

[0038] The tylosin solution was extracted with organic solvent butyl acetate. The extraction adopts two-stage countercurrent extraction, adding 15.7m butyl acetate 3 . During the extraction process, the temperature was controlled at 44-46°C. After the extraction is completed, the raffinate (water phase) titer is 259u / ml; the volume of the ...

Embodiment 3

[0047] Tylosin fermentation broth volume 50m 3 , the potency is 13457u / ml, and the total fermentation value is 673. Control the temperature of the tylosin fermentation broth at 28-30°C, add 20% polyaluminum sulfate solution, adjust the pH of the fermentation broth to 2.9, continue to stir for 15 minutes after polymerization, and control the titer to 13089u / ml after acidification; then use 20% ammonia water Adjust the pH of the fermentation broth, control the pH at 6.9, stir for 15 minutes, let stand for 60 minutes, and filter the fermentation broth with a plate and frame filter to obtain tylosin filtrate 40m 3 , After alkalization, the potency is 16001u / ml.

[0048] The tylosin solution was extracted with organic solvent butyl acetate. The volume of butyl acetate is 18m 3 . During the extraction process, the temperature was controlled at 48-50°C. Use a centrifuge to carry out secondary countercurrent extraction. After the extraction is completed, the raffinate (water phas...

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Abstract

A method for synthesizing tilmicosin and tilmicosin phosphate through using a tylosin broth is disclosed. The method is characterized in that the method comprises the following process steps: preprocessing the tylosin broth to obtain a tylosin filtrate; allowing the tylosin filtrate to undergo extraction, ammonification, reextraction, hydrolysis, acidification liquid extraction and vacuum drying to obtain tilmicosin; and allowing the obtained tilmicosin to undergo phosphorylation and spray drying to obtain tilmicosin phosphate. The method, which directly extracts the tylosin broth which is the initial raw material to synthesize the tilmicosin and the tilmicosin phosphate, allows the production procedure to be simplified, the product production time to be shortened, reaction conditions of the whole technology to be mild, the operation to be simple, the production process to be safe and reliable, and the organic solvent loss to be less, and has the advantages of energy saving and consumption reduction, high finished product yield, low production cost, high working efficiency and the like.

Description

technical field [0001] The invention belongs to the technical field of biomedicine extraction and synthesis, in particular to a method for synthesizing tilmicosin and tilmicosin phosphate by using tylosin fermentation liquid. Background technique [0002] Tilmicosin is a semi-synthetic macrolide antibiotic for livestock and poultry developed by Elanco in the United States in the 1980s. It has strong antibacterial activity, low drug resistance, and a broad antibacterial spectrum. It is effective against all Gram-positive Bacteria and some Gram-negative bacteria, mycoplasma, spirochetes, etc. have inhibitory effects, especially for a variety of mycoplasma and spirochetes. The drug has been approved for clinical use in Australia, Brazil, France, Malaysia, Italy, Spain, the United States and other countries for the treatment of goats, cows, pigs, [0003] Infectious diseases of chickens and other animals. Because tilmicosin is insoluble in water, tilmicosin is phosphorylated a...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/00
Inventor 任勇王文超奇乃纳卓斌
Owner 宁夏泰瑞制药股份有限公司
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