Preparation method and product of ceftriaxone sodium sterile powder

A technology of ceftriaxone sodium and sodium bisulfite, which is applied in the field of medicine, can solve problems such as unfavorable washing and separation, poor crystal form and poor quality of ceftriaxone sodium, achieve shortened production cycle, easy control of reaction conditions, and improve effectiveness Effect

Inactive Publication Date: 2016-10-12
HENAN KANGDA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And mostly use dichloromethane as solvent in production, sodium acetate is salt-forming agent, crystallizes with acetone, but the crystal form of ceftriaxone sodi

Method used

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  • Preparation method and product of ceftriaxone sodium sterile powder
  • Preparation method and product of ceftriaxone sodium sterile powder
  • Preparation method and product of ceftriaxone sodium sterile powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A preparation method of ceftriaxone sodium aseptic powder, comprising the following steps:

[0032] (a) In a clean glass kettle, first cool 12 L of dichloromethane and 1.1 L of ethanol with a mass concentration of 90% to 0-5 °C, then add 0.05 kg of sodium bisulfite, 1.1 kg of AE-activated The ester and 1 kg 7-ACT were dissolved to obtain a mixed solution;

[0033] (b) Add 0.6 kg of triethylamine dropwise to the mixture in step (a) for reaction within 1 hour while maintaining the pH of the system at 8.0 to 8.5 and the temperature at 0 to 5°C. Use HPLC to detect the residual amount of 7-ACT <0.1 %, the reaction is complete;

[0034] (c) After the reaction is finished, add 4.5 kg of sodium bisulfite aqueous solution with a mass concentration of 0.1% for extraction. After the water phase is filtered under reduced pressure, add 5.6 kg of sodium isooctanoate and 2.8 kg sodium acetate reacts into a salt;

[0035] (d) After the salt-forming reaction is complete, add activate...

Embodiment 2

[0037] A preparation method of ceftriaxone sodium aseptic powder, comprising the following steps:

[0038] (a) In a clean glass kettle, first cool 10 L of dichloromethane and 1.2 L of ethanol with a mass concentration of 90% to 0–5°C, then add 0.04 kg of sodium bisulfite, 1.1 kg of AE-activated The ester and 1 kg 7-ACT were dissolved to obtain a mixed solution;

[0039] (b) Add 0.6 kg of triethylamine dropwise to the mixture in step (a) within 1 hour for reaction while maintaining the pH of the system between 8.0 and 8.5 and the temperature at 0 to 5°C. Use HPLC to detect the residual amount of 7-ACT When <0.1%, the reaction is complete;

[0040] (c) After the reaction is over, add 4.2kg of sodium bisulfite aqueous solution with a mass concentration of 0.1% for extraction. After the water phase is filtered under reduced pressure, add 5.7kg of sodium isooctanoate and 2.8 kg sodium acetate reacts into a salt;

[0041] (d) After the salt-forming reaction is complete, add activ...

Embodiment 3

[0043] A preparation method of ceftriaxone sodium aseptic powder, comprising the following steps:

[0044] (a) In a clean glass kettle, first cool 12 L of dichloromethane and 1.2 L of ethanol with a mass concentration of 90% to 0-5°C, then add 0.05 kg of sodium bisulfite, 1.05 kg of AE-active The ester and 1 kg 7-ACT were dissolved to obtain a mixed solution;

[0045] (b) Add 0.65 kg of triethylamine dropwise to the mixture in step (a) for reaction within 1 hour while maintaining the pH of the system between 8.0 and 8.5 and the temperature at 0 to 5°C. Use HPLC to detect the residual amount of 7-ACT When <0.1%, the reaction is complete;

[0046](c) After the reaction is over, add 4.4kg of sodium bisulfite aqueous solution with a mass concentration of 0.1% for extraction. After the water phase is filtered under reduced pressure, add 5.5kg of sodium isooctanoate and 2.8 kg sodium acetate reacts into a salt;

[0047] (d) After the salt-forming reaction is complete, add activat...

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Abstract

The invention discloses a preparation method of ceftriaxone sodium sterile powder, and belongs to the technical field of medicine. The method comprises the following steps of mixing methylene dichloride and alcohol; lowering the temperature; sequentially adding antioxidizers, 7-ACT and AE-active esters; dissolving the materials to obtain a mixed solution; dripping triethylamine into the mixed solution within 1h for reaction; performing extraction after the reaction is completed; after the pressure reduction suction filtration on a water phase, adding a salt forming agent for reaction and salt forming; after a decoloring agent is added into a salt forming reaction solution, performing sterile filtration; adding a solvating agent into filter liquid for crystallization; performing post-treatment to obtain the ceftriaxone sodium sterile powder. The preparation method has the advantages that the operation is simple; the reaction conditions are mild; the control is easy; the ceftriaxone sodium sterile powder is prepared in one step; the refining process is omitted; the production period is shortened; the cost is greatly reduced; the quality yield reaches 165 percent or higher; the product purity can reach 99.5 percent or higher.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method and product of ceftriaxone sodium sterile powder. Background technique [0002] Ceftriaxone sodium (Ceftriaxone sodium), the chemical name is {6R[6α,7β(2)]}-3-{[1,2,5,6-tetrahydro-2-methyl-5,6-dioxide -1,2,4-Triazin-3-yl)thio]methyl}-7-{[(2-amino-4-thioxime)(methylimino)acetyl]amino}-β- Oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid disodium salt triple hemihydrate is the third-generation cephalosporin widely used in clinical practice Compared with other cephalosporins, ceftriaxone sodium has the following significant advantages: 1) The bactericidal effect mainly inhibits the synthesis of bacterial cell walls, and human cells do not have cell walls, so they are less affected, so the relative toxicity is relatively low; 2) Long half-life, one-time administration The drug can play an antibacterial effect within 24 hours; 3) It has a br...

Claims

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Application Information

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IPC IPC(8): C07D501/04C07D501/12C07D501/36A61K9/14A61P31/04
CPCC07D501/04A61K9/14C07D501/12C07D501/36
Inventor 孙津鸽李红德李文杰李志军高德瀛刘红坤白金钟
Owner HENAN KANGDA PHARMA
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