Method for preparing injection-grade oxytetracycline
A technology of oxytetracycline and injection grade is applied in the field of preparation of injection grade oxytetracycline to achieve the effects of reducing types and contents, qualified quality standards and lowering production costs
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example 1
[0031] (1) Dissolve 10 grams of oral grade oxytetracycline in 200ml of methanol, slowly add methanol-hydrochloric acid solution dropwise until dissolved, stir for 10 minutes, add 2.0g of 767 carbon powder, stir for 20 minutes, carry out coarse filtration, and then carry out membrane Filtrate, add methanol-hydrochloric acid solution to the filtrate at 10°C-30°C to adjust pH = 1-2, crystallize at 20°C-25°C for 3 hours, and filter with suction to obtain the wet product of oxytetracycline hydrochloride;
[0032] (2) Dissolve the wet product of oxytetracycline hydrochloride in purified water, stir for 10 minutes, filter the solution with a membrane, and wash the upper layer with purified water until the effluent is colorless, combine the filtrates, and store at 20-25°C Slowly add 10% sodium hydroxide solution dropwise under stirring, adjust the pH to 5-6 to obtain oxytetracycline base crystals, stir for 15 minutes, filter, wash the upper layer with purified water until the effluent ...
example 2
[0036] (1) Dissolve 10g of oral grade oxytetracycline in 150ml of methanol, slowly add methanol-hydrochloric acid solution dropwise until dissolved, stir for 15 minutes, add 1.5g of 767 carbon powder, stir for 20 minutes, carry out coarse filtration, and then perform membrane Filtrate, add methanol-hydrochloric acid solution to the filtrate at 10°C to 30°C to adjust pH=1 to 2, crystallize at 15°C to 20°C for 4 hours, and filter with suction to obtain the wet product of oxytetracycline hydrochloride;
[0037] (2) Dissolve the wet product of oxytetracycline hydrochloride in purified water, stir for 15 minutes, filter the solution with a membrane, and wash the upper layer with purified water until the effluent is colorless. Slowly add 10% sodium hydroxide solution dropwise under stirring at ℃, adjust the pH to 5-6 to obtain oxytetracycline base crystals, stir for 15 minutes, filter, wash the upper layer with purified water until the effluent is neutral, filter and dry to obtain ox...
example 3
[0041] (1) Dissolve 10 grams of oral grade oxytetracycline in 120ml of methanol, slowly add methanol-hydrochloric acid solution dropwise until dissolved, stir for 15 minutes, add 0.8g of 767 carbon powder, stir for 20 minutes, perform coarse filtration, and then perform membrane Filtrate, add methanol-hydrochloric acid solution to the filtrate at 10°C-30°C to adjust pH = 1-2, crystallize at 5°C-10°C for 5 hours, and filter with suction to obtain the wet product of oxytetracycline hydrochloride;
[0042] (2) Dissolve the wet product of oxytetracycline hydrochloride in purified water, stir for 20 minutes, filter the solution with a membrane, after filtration, wash with purified water until the effluent is colorless, combine the filtrates, and stir at 10°C to 15°C Slowly add 10% sodium hydroxide solution dropwise to adjust the pH to 5-6 to obtain oxytetracycline base crystals, stir for 15 minutes, filter, wash the upper layer with purified water until the effluent is neutral, and ...
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