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Purification method of cefazolin sodium

A technology of cefazolin sodium and a purification method, which is applied in the field of purification of cefazolin sodium, can solve the problems of degradation and new impurity generation, heavy environmental protection treatment burden, complicated operation and the like, and achieves reduction of waste water consumption, drug safety and high content Effect

Inactive Publication Date: 2019-11-22
石药集团中诺药业(石家庄)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The operation is cumbersome, problems in the intermediate links will easily lead to quality deviation, a large amount of waste water will be generated, and the environmental protection treatment burden will be heavy, and the long operation cycle will easily lead to degradation and new impurities.
Other methods such as purification with resin columns are similar, and have the same problems and defects as alumina columns.

Method used

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  • Purification method of cefazolin sodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] After the synthesis of cefazolin is completed, after adding water for hydrolysis, add 100ml of hydrolyzed solution containing 2g of cefazolin acid, add 50ml of dichloromethane, add 10% hydrochloric acid dropwise while stirring, control pH=1.3~1.6, and then let it stand for 10 minute. Separate the phases, discard the water phase, collect the dichloromethane phase, add 100ml of water, stir, adjust the pH to 6.4-6.7 with 10% sodium hydroxide solution, and let stand for 10 minutes. The phases were separated, and the dichloromethane phase was discarded to obtain a purified cefazolin sodium solution with a yield of 92.4%, a content of 98.1%, and a single compound of 0.21%. The purified cefazolin sodium solution is crystallized to obtain pure cefazolin sodium; the crystallization solvent is acetone; the volume of the crystallization solvent is 3 times the volume of the cefazolin sodium solution; and the crystallization temperature is 10-15°C.

Embodiment 2

[0030] After the synthesis of cefazolin is completed, after adding water for hydrolysis, add 100ml of hydrolyzed solution containing 2.5g of cefazolin acid, add 80ml of dichloromethane, add 12% hydrochloric acid dropwise while stirring, control the pH=1.3~1.6, and then let stand 10 minutes. Separate the phases, discard the water phase, collect the dichloromethane phase, add 150ml of water, stir, adjust the pH to 6.4-6.7 with 10% sodium hydroxide solution, and let stand for 10 minutes. The phases were separated, and the dichloromethane phase was discarded to obtain a purified cefazolin sodium solution with a yield of 93.0%, a content of 98.2%, and a single compound of 0.23%. The purified cefazolin sodium solution is crystallized to obtain pure cefazolin sodium; the crystallization solvent is acetone; the volume of the crystallization solvent is 4 times the volume of the cefazolin sodium solution; and the crystallization temperature is 10-15°C.

Embodiment 3

[0032] After the synthesis of cefazolin is completed, after adding water for hydrolysis, add 100ml of hydrolyzed solution containing 1.5g of cefazolin acid, add 100ml of dichloromethane, add 8% hydrochloric acid dropwise while stirring, control the pH=1.3~1.6, and then let stand 10 minutes. Separate the phases, discard the water phase, collect the dichloromethane phase, add 120ml of water, stir, adjust the pH to 6.4-6.7 with 8% sodium hydroxide solution, and let stand for 10 minutes. The phases were separated, and the dichloromethane phase was discarded to obtain a purified cefazolin sodium solution with a yield of 88%, a content of 98.6%, and a single compound of 0.15%. The purified cefazolin sodium solution is crystallized to obtain pure cefazolin sodium; the crystallization solvent is acetone; the volume of the crystallization solvent is 5 times the volume of the cefazolin sodium solution; and the crystallization temperature is 10-15°C.

[0033] The existing purification m...

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Abstract

The invention discloses a purification method of cefazolin sodium, and relates to the technical field of purification of cefazolin sodium. The method comprises the following steps: (1) after cefazolinis synthesized, adding water for hydrolysis, adding dichloromethane into hydrolysate, then adding hydrochloric acid, controlling the pH value to be 1.3-1.6, standing, carrying out phase splitting, discarding a water phase, and collecting a dichloromethane phase; and (2) adding water into the dichloromethane phase, adjusting the pH value to 6.4-6.7 by using a sodium hydroxide solution, standing, carrying out phase splitting, and discarding the dichloromethane phase to obtain a purified cefazolin sodium solution. The method disclosed by the invention is simple and convenient to operate, short in period and less in wastewater discharge, and has the advantage of environmental protection, and the product cefazolin sodium is high in content, less in impurity variety, low in impurity content andsafe to use as medicine.

Description

technical field [0001] The invention relates to the technical field of purification of cefazolin sodium. Background technique [0002] Cefazolin is a first-generation cephalosporin with a broad antibacterial spectrum. Except for Enterococcus and methicillin-resistant Staphylococcus, this product has good antibacterial activity against other Gram-positive cocci. Streptococcus pneumoniae and hemolytic streptococcus are highly sensitive to this product. Diphtheria, Bacillus anthracis, Listeria and Clostridium are also very sensitive to this product. This product has good antibacterial activity against some Escherichia coli, Proteus mirabilis and Klebsiella pneumoniae, but has poor antibacterial activity against Staphylococcus aureus. Salmonella typhi, Shigella and Neisseria are sensitive to this product, and other Enterobacteriaceae, Acinetobacter and Pseudomonas aeruginosa are resistant. Neisseria gonorrhoeae are resistant to this product; Haemophilus influenzae is only mod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/12
CPCC07D501/12C07D501/36
Inventor 徐永龙魏青杰李世成黄学川邱增会郝乐谢子龙
Owner 石药集团中诺药业(石家庄)有限公司
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