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
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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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