Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Separation and purification method of cefminox sodium and preparation of cefminox sodium freeze-dried powder injection

A technology of cefminox sodium and freeze-dried powder injection, which is applied in the field of medicine, can solve the problems of many foreign substances, unstable aqueous solution, and low purity, and achieve the effects of large separation, avoiding sample loss, and saving solvents

Inactive Publication Date: 2008-10-08
HAINAN LINGKANG PHARMA CO LTD
View PDF0 Cites 8 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most cefminox sodium has the problem of low purity, many foreign substances can be seen after dissolution, and the aqueous solution is extremely unstable, which is also a common problem of all antibiotic drugs
[0004] High-Speed ​​Countercurrent Chromatography (High-Speed ​​Countercurrent Chromatography) is a continuous and high-efficiency liquid-liquid partition chromatography separation technology. Because it uses a liquid stationary phase and does not require a solid support, it avoids sample loss, inactivation and denaturation caused by irreversible adsorption. etc., have developed very rapidly in the past 20 to 30 years, but there is no report that high-speed countercurrent chromatography is used for the separation and purification of cefminox sodium

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 cefminox sodium and preparation of cefminox sodium freeze-dried powder injection
  • Separation and purification method of cefminox sodium and preparation of cefminox sodium freeze-dried powder injection
  • Separation and purification method of cefminox sodium and preparation of cefminox sodium freeze-dried powder injection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A semi-preparative high-speed countercurrent chromatograph is used, equipped with a constant flow pump, a 15ml injection valve, a polytetrafluoroethylene column with a column volume of 200ml, and a UV ultraviolet detector. Mix chloroform with a volume ratio of 1:1.2:1: methanol: water in a separatory funnel, shake it up and let it stand to separate layers, take its upper layer solution (upper phase) as the stationary phase, and the lower layer solution (lower phase) ) as the mobile phase, after ultrasonic degassing, first fill the entire column with the stationary phase, then turn on the high-speed countercurrent chromatograph, adjust the host speed to 900rpm, pump the mobile phase into the column at a flow rate of 1.3ml / min, and wait until the entire system After the dynamic equilibrium is established, the cefminox sodium raw material is dissolved in the lower phase, and the sample is injected through the injection valve, and then according to the ultraviolet spectrum o...

Embodiment 2

[0027] A semi-preparative high-speed countercurrent chromatograph is used, equipped with a constant flow pump, a 15ml injection valve, a polytetrafluoroethylene column with a column volume of 200ml, and a UV ultraviolet detector. Mix chloroform with a volume ratio of 0.8:1.4:1: Methanol: water in a separatory funnel, shake well and let stand to separate layers, take its upper layer solution (upper phase) as the stationary phase, and the lower layer solution (lower phase) ) as the mobile phase, after ultrasonic degassing, first fill the entire column with the stationary phase, then turn on the high-speed countercurrent chromatograph, adjust the speed of the main engine to 1200rpm, and pump the mobile phase into it at a flow rate of 1.3ml / min, and wait until the entire system is established After dynamic equilibrium, dissolve the cefminox sodium raw material in the lower phase, inject the sample through the injection valve, and then collect and collect more than 98% of the part a...

Embodiment 3

[0031] A semi-preparative high-speed countercurrent chromatograph is used, equipped with a constant flow pump, a 15ml injection valve, a polytetrafluoroethylene column with a column volume of 200ml, and a UV ultraviolet detector. Mix chloroform:methanol:water with a volume ratio of 0.5:1.5:1 in a separatory funnel, shake it up and let it stand for layering, take its upper layer solution (upper phase) as the stationary phase, and the lower layer solution (lower phase) ) as the mobile phase, after ultrasonic degassing, first fill the entire column with the stationary phase, then turn on the high-speed countercurrent chromatograph, adjust the host speed to 1000rpm, pump the mobile phase into the column at a flow rate of 1.2ml / min, and wait for the entire system to After the dynamic equilibrium is established, the cefminox sodium raw material is dissolved in the lower phase, and the sample is injected through the injection valve, and then according to the ultraviolet spectrum of th...

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

The invention discloses a method to separate and purify cefminox sodium. Solvent is prepared from trichloromethane, ethyl acetate, carbinol and water, with the upper phase being stationary and the lower phase being mobile. The whole column of a high-speed countercurrent chromatograph is filled with stationary phase solvent and then the mobile phase solvent is pumped into the column; the raw material of cefminox sodium is dissolved in the solvent at the lower phase and the material is fed by an injection valve; above 98% of the product is collected according to the map of the detector and then the solvent is removed to obtain refined cefminox sodium. The method is good in effect and the product is of high purity. The cefminox sodium can be further froze and dried to prepare freeze-dried powder injection. The method is good in separation effect and the product is of high purity.

Description

technical field [0001] The invention belongs to the field of medicine, and specifically relates to a separation and purification method of cefminox sodium and a preparation method of cefminox sodium freeze-dried powder injection. Background technique [0002] Cefminox sodium has broad-spectrum antibacterial activity against Gram-positive bacteria and Gram-negative bacteria, especially against Escherichia coli, Klebsiella, Haemophilus influenzae, Proteus and Bacteroides fragilis effect. Its mechanism of action is that it has a strong affinity for the penicillin-binding protein at the usual site of action of β-lactam antibiotics, can inhibit the synthesis of cell walls, and bind to peptidoglycan, inhibiting the combination of peptidoglycan and lipoprotein to promote bacteriolysis. Shows strong bactericidal power in a short time. This product is suitable for respiratory system infection, urinary system infection, abdominal infection, pelvic infection and sepsis caused by sens...

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 朱正兵
Owner HAINAN LINGKANG PHARMA CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com