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Method for removing bacterial endotoxins in cephalosporin antibiotics by utilizing macroporous adsorption resins

A technology of bacterial endotoxin and cephalosporin, applied in the field of separation, to achieve the effect of less adsorption, small fluid resistance and easy amplification

Inactive Publication Date: 2011-03-02
东瑞(南通)医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Macroporous adsorption resin has not been reported in the removal of bacterial endotoxin by antibiotics

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Obtain the cefotaxime triethylamine salt solution that 1200L bacterial endotoxin is greater than 0.05EU / mg by reaction, pH value 8.0, after plate and frame filter press filter removes solid insolubles, enter with pressure (2 atmospheres) into containing 100kg (wet) Heavy) DM1180 macroporous adsorption resin packed column for dynamic adsorption treatment. After the treatment, the resin can be further washed with water. Regulate pH to 3.5 with hydrochloric acid through the filtrate of resin treatment, crystallization obtains cefotaxime acid, after drying, pulverizing, obtain 240kg bacterial endotoxin less than 0.05EU / mg cefotaxime acid, the loss rate of cefotaxime acid is lower than 0.5% .

Embodiment 2

[0038] Obtain 40L bacterial endotoxin greater than 0.05EU / mg cefotaxime triethylamine salt solution by reaction, pH8.0, after plate and frame filter press filter removes solid insoluble matter, enter under normal pressure and contain 3.5kg (wet weight) The packed column of DM1180 macroporous adsorption resin is used for dynamic adsorption treatment. Regulate pH to 3.5 with hydrochloric acid through the filtrate of resin treatment, crystallization obtains cefotaxime acid, after drying, pulverizing, obtain 8kg, the cefotaxime acid that bacterial endotoxin is less than 0.05EU / mg, the loss rate of cefotaxime acid is lower than 1 %.

Embodiment 3

[0040] Obtain 100L bacterial endotoxin greater than the ceftriaxone triethylamine salt solution of 0.15EU / mg by reaction, pH8.0, after plate and frame filter press filter removes solid insolubles, enter with pressure (2 atmospheres) into containing 3.5Kg ( Wet weight) DM1180 macroporous adsorption resin packed column for dynamic adsorption treatment. After the treatment, the resin is washed with a mixed solution of water and organic solvent. Filtrate adds sodium acetate solution, and adds acetone, and crystallization obtains ceftriaxone sodium, obtains 15kg after drying, pulverizing, and bacterial endotoxin is less than the ceftriaxone sodium of 0.15EU / mg, and the loss rate of ceftriaxone sodium is lower than 1%.

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PUM

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Abstract

The invention discloses a method for removing bacterial endotoxins in cephalosporin antibiotics by utilizing macroporous adsorption resins, comprising the following steps: firstly filtering the cephalosporin antibiotics solution containing the bacterial endotoxins and removing solid insoluble matters; then utilizing the pretreated macroporous adsorption resins to carry out static adsorption or dynamic adsorption on the cephalosporin antibiotics solution; and finally crystallizing, drying and grinding the solution after adsorption treatment, thus obtaining the product with bacterial endotoxins in accordance with the quality standard. The method has the advantages of high bacterial endotoxins removal rate, good selectivity, easy desorption, repeated use, low fluid resistance and easy magnification.

Description

technical field [0001] The invention belongs to the technical field of separation, and in particular relates to a method for removing bacterial endotoxins in cephalosporin antibiotics with a macroporous adsorption resin. Background technique [0002] Bacterial endotoxin is a unique structure on the outer membrane of the cell wall of Gram-negative bacteria. Its essence is lipopolysaccharide, and its chemical structure is mainly composed of two major parts, namely polysaccharide and lipid A. Lipid A is the active center of lipopolysaccharide, mainly composed of glucosamine and long fatty acids with 10-18 carbon phosphates, and has hydrophobicity and electronegativity under the condition of cephalosporin salt solution. A very small amount of endotoxin entering the human body will cause high fever, diarrhea, dilation of blood vessels, and even fainting or death. [0003] Since manufacturers of upstream raw materials of cephalosporin antibiotics have adopted enzymatic processes ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/12C07D501/34C07D501/36C07D501/46C07D501/57
Inventor 张西峰陈永生施新华施袁园邵建良
Owner 东瑞(南通)医药科技有限公司
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