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
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  • 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 sep

Method used

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  • 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
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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...

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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

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Application Information

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IPC IPC(8): C07D501/36A61K31/546A61K9/19A61P31/04
Inventor 朱正兵
Owner HAINAN LINGKANG PHARMA CO LTD
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