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A kind of purification method of cefpirome sulfate

A technology of cefpirome sulfate and a purification method, which is applied in the field of medicine, can solve the problems of complex operation, high cost, and unsuitability for large-scale application, and achieve the effect of low process cost, low cost, and easy control

Active Publication Date: 2020-01-21
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a purification method of cefpirome sulfate, to solve the problems of high cost, complex operation and unsuitable large-scale application of existing methods

Method used

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  • A kind of purification method of cefpirome sulfate
  • A kind of purification method of cefpirome sulfate
  • A kind of purification method of cefpirome sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 240 mL of purified water to the reaction tank, add 47.4 g of cefpirome sulfate sodium carbonate mixed powder (containing 40.0 g of pure pirome) under stirring, stir until it dissolves, then add sulfuric acid with a mass concentration of 15% to adjust the pH of the system to 5.5 , control the temperature of the system at 0°C, add 600mL of acetone, stir and precipitate white sodium sulfate crystals, and after stirring for 90min, filter the solution to remove salt.

[0026] Add activated carbon 4.0g to the filtrate and stir for 90min before filtering, after filtration, add mass concentration to the filtrate to adjust the system pH=0.5 with sulfuric acid aqueous solution with a mass concentration of 15%, add activated carbon 4.0g again and stir for 60min before filtering, after aseptic filtration, the filtrate enters The crystallization tank was washed with a mixture of 20 mL of purified water and 50 mL of acetone, and combined into the crystallization tank.

[0027] Co...

Embodiment 2

[0029] Add 400 mL of purified water to the reaction tank, add 47.4 g of cefpirome sulfate sodium carbonate mixed powder (containing 40.0 g of pure Piro) under stirring conditions, stir until it dissolves, then add sulfuric acid with a mass concentration of 98% to adjust the pH of the system to 3.8 , control the temperature of the system at 0°C, add 1200mL of acetone, stir and precipitate white sodium sulfate crystals, and after stirring for 90min, filter the solution to remove salt.

[0030] Add activated carbon carbon 6.0g to the filtrate and filter after stirring for 60min, add mass concentration to the filtrate after filtering and add a sulfuric acid aqueous solution that is 15% to adjust the system pH=1.0, add activated carbon again 8.0g and stir after 60min to filter, after aseptic filtration, the filtrate Enter the crystallization tank, wash with a mixture of 20mL purified water and 50mL acetone, and combine it into the crystallization tank.

[0031] Control the crystall...

Embodiment 3

[0033] In reaction tank, add purified water 240L, add cefpirome sulfate sodium carbonate mixed powder 47.4kg (containing pirome pure product 40kg) under stirring condition, after stirring to dissolving clear, adding mass concentration is that the sulfuric acid adjustment system pH=4.5 of 40%, Control the temperature of the system at 2°C, add a mixed solution consisting of 600L of acetone, 70L of ethanol, and 50L of isobutanol, and stir to precipitate white sodium sulfate crystals. After stirring for 60 minutes, filter the solution to remove salt.

[0034] Add 4.0 kg of activated carbon to the filtrate and stir for 60 minutes before filtering, add sulfuric acid with a mass concentration of 40% to the filtrate to adjust the pH of the system to 0.86, add 4.0 kg of activated carbon and stir for 60 minutes before filtering, after sterile filtration, the filtrate enters the crystallization tank , washed with 20L of purified water and 50L of acetone mixture, and combined into a crysta...

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Abstract

The invention provides a purifying method of cefpirome sulfate. The purifying method comprises the following steps: (a) dissolving unqualified cefpirome sulfate and sodium carbonate mixed powder intowater, and regulating pH (Potential of Hydrogen) to be 3.8 to 5.5 by using a sulfuric acid water solution after dissolving and clarifying; (b) adding an organic solvent in a solution obtained in step(a), reducing the temperature to 0 to 5 DEG C, stirring for desalting, and filtering; (c) adding activated carbon in filtrate obtained in step (b) for first decoloring, and filtering after decoloring;(d) regulating the pH of the filtrate obtained in step (c) to be 0.5 to 1.0 by using the sulfuric acid water solution, then adding the activated carbon for second decoloring, and filtering after decoloring; (e) crystallizing. The purifying method disclosed by the invention is simple in operation, easy to control and low in cost; through a special desalting technology and special decoloring technology, the purifying method has high ability of removing sodium sulfate, does not need to pass an adsorption column. The obtained cefpirome sulfate through purification provided by the invention has the advantages of good stability, low color grade index and high content.

Description

technical field [0001] The invention belongs to the technical field of medicine, in particular to a method for purifying cefpirome sulfate. Background technique [0002] Cefpirome is a fourth-generation cephalosporin with broad-spectrum antibacterial activity, effective against staphylococci, penicillin-resistant pneumococci and enterococci, and has good curative effects against many antibiotic-resistant pathogens. It is known as the third-generation and Among the fourth-generation cephalosporins, it is the antibiotic with the strongest antibacterial activity against Gram-positive bacteria. The sulfate salt of cefpirome is well absorbed in the stomach, so cefpirome is usually prepared in the sulfate form. Because cefpirome sulfate itself is slightly soluble in water and is acidic, it is generally used as an injection after being mixed with sodium carbonate for clinical use. The chemical name of cefpirome sulfate is: 1-[[7-[[(2-amino-4-thiazolyl)(methoxyimino)acetyl]-amino]...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/46
CPCC07D501/46
Inventor 田洪年张锁庆石春利李庆伟贾全刘树斌任峰贺娇
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA