A kind of anti-infection drug ceftazidime crystal compound and its pharmaceutical composition
A crystalline compound, a technology for ceftazidime, applied in the field of medicine, can solve the problems of difficult and accurate quantification of ceftazidime, increased risk of adverse reactions, large differences in loading, etc., and achieves low pyridine and polymer content, good clarity, and different loadings. small effect
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Embodiment 1
[0041] The preparation of embodiment 1 ceftazidime crystal compound
[0042] 1) Dissolving the ceftazidime crude product in a mixed solvent A of ethanol and water whose volume is 6 times the weight of ceftazidime at 15°C, the volume ratio of ethanol to water is 1:2.5;
[0043] 2) First add the mixed solvent B of N-methylpyrrolidone and dichloromethane whose total volume is 6 times the weight of ceftazidime at a speed of 20ml / min, and the volume ratio of N-methylpyrrolidone and dichloromethane is 1:4 , Stir while adding, control the temperature at 15°C, and grow the crystal for 0.5 hours;
[0044] 3) Add the mixed solvent C of N-methylpyrrolidone and dichloromethane whose total volume is 9 times the weight of ceftazidime at a speed of 12ml / min, and the volume ratio of N-methylpyrrolidone and dichloromethane is 1:3 , after growing the crystal for 4 hours, lower the temperature to -5°C at a rate of 20°C / hour, then stir and crystallize, and grow the crystal for 2 hours;
[0045]...
Embodiment 2
[0053] The preparation of embodiment 2 ceftazidime crystal compound
[0054] 1) Dissolving the ceftazidime crude product in a mixed solvent A of ethanol and water whose volume is 8 times the weight of ceftazidime at 10° C., the volume ratio of ethanol to water is 1:2.5;
[0055] 2) First add the mixed solvent B of N-methylpyrrolidone and dichloromethane whose total volume is 7 times the weight of ceftazidime at a speed of 15ml / min, and the volume ratio of N-methylpyrrolidone and dichloromethane is 1:4 , Stir while adding, control the temperature at 25°C, and grow the crystal for 0.5 hours;
[0056] 3) Add the mixed solvent C of N-methylpyrrolidone and dichloromethane whose total volume is 10 times the weight of ceftazidime at a speed of 10ml / min, and the volume ratio of N-methylpyrrolidone and dichloromethane is 1:3 , after growing the crystal for 5 hours, lower the temperature to -5°C at a rate of 15°C / hour, then stir and crystallize, and grow the crystal for 1 hour;
[005...
Embodiment 3
[0059] The preparation of embodiment 3 ceftazidime crystal compound
[0060] 1) Dissolving the ceftazidime crude product in a mixed solvent A of ethanol and water whose volume is 4 times the weight of ceftazidime at 25° C., the volume ratio of ethanol to water is 1:2.5;
[0061] 2) First add the mixed solvent B of N-methylpyrrolidone and dichloromethane whose total volume is 5 times the weight of ceftazidime at a speed of 24ml / min, and the volume ratio of N-methylpyrrolidone and dichloromethane is 1:4 , Stir while adding, control the temperature at 10°C, and grow the crystal for 1 hour;
[0062] 3) Add the mixed solvent C of N-methylpyrrolidone and dichloromethane whose total volume is 8 times the weight of ceftazidime at a speed of 15ml / min, and the volume ratio of N-methylpyrrolidone and dichloromethane is 1:3 , after growing crystals for 2 hours, cool down to -5°C at a rate of 20°C / hour, then stir and crystallize, and grow crystals for 3 hours;
[0063] 4) Filtration, was...
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