Separation and purification method of cefamandole nafate and preparation of cefathiamidine freeze-dried injectable powder

A technology for the separation and purification of cefamandole sodium, which is applied in freeze-dried transportation, medical preparations containing active ingredients, organic chemistry, etc. It can solve problems such as poor clarity, low purity, and poor stability, and achieve improved purity , the effect of improving solubility

Inactive Publication Date: 2008-10-08
HAINAN LINGKANG PHARMA CO LTD
View PDF0 Cites 18 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most cefamandole sodium raw materials have the problems of low purity, poor clarity after dissolution,

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Separation and purification method of cefamandole nafate and preparation of cefathiamidine freeze-dried injectable powder
  • Separation and purification method of cefamandole nafate and preparation of cefathiamidine freeze-dried injectable powder
  • Separation and purification method of cefamandole nafate and preparation of cefathiamidine freeze-dried injectable powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Cefamandole sodium raw material loading amount 200mg, purity 95.8%. Solvent system: chloroform, ethyl acetate, methanol, water volume ratio 2:2.5:1.8:1 (volume ratio), column volume: 200ml, rotating speed 800rpm, upper phase is stationary phase, lower phase is mobile phase, flow rate 2ml / min, stationary phase retention: 52%.

[0019] Prepare a solvent system according to the volume ratio of chloroform, ethyl acetate, methanol, and water in a ratio of 2:2.5:1.8:1, let it stand for stratification, separate the upper and lower phases, take the upper phase as the stationary phase, and the lower phase as the mobile phase. Make the high-speed countercurrent chromatograph column full of stationary phase, then make the main engine rotate clockwise, then pump the mobile phase into the column, dissolve the cefamandole sodium raw material with the lower phase solvent, and then inject the sample through the injection valve. The spectrum receives the target components.

[002...

Embodiment 2

[0026] Get cefamandole sodium raw material, operation step is by embodiment 1, and difference is: in step (1), solvent system: the volume ratio of chloroform, ethyl acetate, methyl alcohol, water is 1.5: 1.8: 1: 1 , solvent system in step (2): chloroform: ethyl acetate: methanol: the volume ratio of water is 1.0: 0.8: 1.3: 1, solvent system in step (3): chloroform: ethyl acetate: methanol: The volume ratio of water is 0.8:0.5:1.0:1. After purification, the purity is 99.3% as detected by high performance liquid chromatography. Aseptic subpackaging to obtain a sterile preparation of cefamandole sodium freeze-dried powder for injection.

Embodiment 3

[0028] Get cefamandole sodium raw material, operation step is by embodiment 1, and difference is: in step (1), solvent system: the volume ratio of chloroform, ethyl acetate, methyl alcohol, water is 3.0: 3.5: 2.5: 1 , solvent system in step (2): chloroform: ethyl acetate: methanol: the volume ratio of water is 2.5: 2.0: 1.5: 1, solvent system in step (3): chloroform: ethyl acetate: methanol: The volume ratio of water is 0.5:1.0:0.7:1. After purification, the purity detected by high performance liquid chromatography was 97.2%. Aseptic subpackaging to obtain a sterile preparation of cefamandole sodium freeze-dried powder for injection.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

Disclosed is a method to separate and purify cefamandole nafate, which is characterized in that cefamandole nafate is separated and purified for three times through a high-speed countercurrent chromatograph which adopts a solvent system composed of trichloromethane, ethyl acetate, carbinol and water, with the upper phase being stationary and the lower phase being mobile. The cefamandole nafate can be further froze and dried to prepare freeze-dried powder injection. The method greatly increases the purity of the material up to 99%, and the purification process causes no pollution; therefore the method is good for industrial continuous production.

Description

technical field [0001] The invention relates to a separation and purification method of cefamandole sodium and a preparation method of cefamandole sodium freeze-dried powder preparation. Background technique [0002] Cefamandole sodium is a second-generation cephalosporin antibiotic, and cefamandole sodium enters the body and is rapidly hydrolyzed into cefamandole. It is suitable for lung infection, urinary tract infection, biliary tract infection, skin and soft tissue infection, bone and joint infection, sepsis and abdominal infection caused by sensitive bacteria. [0003] Cefamandole sodium powder for injection has been widely used clinically, with definite curative effect and good market prospect, and its preparations are all prepared by aseptic subpackaging of cefamandole sodium raw materials. Most cefamandole sodium raw materials have the problems of low purity, poor clarity after dissolution, and poor stability in aqueous solution, which is also a common problem of al...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07D501/36A61K31/546A61K9/19A61P31/04
Inventor 王明
Owner HAINAN LINGKANG PHARMA CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap