Method for producing high-purity azlocillin sodium and powder injection thereof

A technology of azlocillin sodium powder and azlocillin sodium, applied in the field of medicine, can solve the problems of low purity, poor stability, poor clarity and the like, and achieve the effects of high purity, low cost and improved stability

Inactive Publication Date: 2008-09-17
海南华旗药业销售有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most azlocillin sodium raw materials have problems of low purity, poor clarity after dissolution, and poor stability in aqueous solution, which is also a common problem of all antibiotic drugs

Method used

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  • Method for producing high-purity azlocillin sodium and powder injection thereof
  • Method for producing high-purity azlocillin sodium and powder injection thereof
  • Method for producing high-purity azlocillin sodium and powder injection thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 500g of crude azlocillin sodium was stirred and dissolved in 2L of purified water, added hydrochloric acid to adjust the pH to 1, and extracted with 6L of dichloromethane three times, the extract was dehydrated through an anhydrous sodium sulfate column, and then concentrated to dryness under reduced pressure. After suspending 5kg of 50-mesh alumina with activity level II in n-hexane, remove the air bubbles, and evenly add it to a glass chromatography column with an effective column length of 20cm and an inner diameter of 5cm, and add 600ml of the crude azlocillin sodium concentrated above The eluent (the mass ratio of normal hexane to dichloromethane is 1:99) is dissolved, and the insoluble matter is filtered out and put on the column head with a plunger solvent pump, and then the eluent is pumped in (the mass ratio of normal hexane to dichloromethane is 1:99). 1:99) elution, column pressure is 0.1MPa, segmental collection fraction, TLC and HPLC detection, merge the eff...

Embodiment 2

[0043] 500g of crude azlocillin sodium was stirred and dissolved in 2L of purified water, added sulfuric acid to adjust the pH to 6, extracted with 8L of n-butanol, the extract was dehydrated through an anhydrous magnesium sulfate column, and then concentrated to dryness under reduced pressure. Suspend 100 kg of 800 mesh alumina with activity level II in n-hexane, remove air bubbles, and evenly add it to a glass chromatography column with an effective column length of 2000 cm and an inner diameter of 100 cm, and add the crude azlocillin sodium concentrated to dryness 700ml of eluent (cycloheptane and chloroform mass ratio is 100:1) is dissolved, and the insoluble matter is filtered off and put on the column head with a plunger solvent pump, and then pumped into the eluent (cycloheptane and chloroform The mass ratio is 100:1) elution, the column pressure is 5MPa, the fractions are collected in sections, detected by TLC and HPLC, the effluent with azlocillin acid content greater ...

Embodiment 3

[0045] 500g of crude azlocillin sodium was stirred and dissolved in 2L of purified water, added phosphoric acid to adjust the pH to 2, extracted with 7L of cyclooctane, the extract was dehydrated through an anhydrous calcium chloride column, and then concentrated to dryness under reduced pressure. After suspending 7.5kg of 100-mesh alumina with activity level II with n-hexane, remove air bubbles, and evenly add it to a glass chromatography column with an effective column length of 30cm and an inner diameter of 10cm. The crude azlocillin sodium concentrated to dry Add 650ml of eluent (the mass ratio of 1-nonene to 1,2-dichloroethane is 1:4) to dissolve, filter out the insoluble matter and put it on the column head with a plunger solvent pump, then pump the eluent ( The mass ratio of 1-nonene to 1,2-dichloroethane is 1:4), and the column pressure is 2.5MPa. The fractions are collected in sections, detected by TLC and HPLC, and the combined azlocillin acid content is greater than ...

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Abstract

The invention provided a method for preparing high-purity Mezlocillin sodium, and a method for preparing the Mezlocillin sodium powder injection. The method includes (1) dissolving Mezlocillin sodium crude product in purified water, and adjusting the pH value to less than 7 with the pH regulator; (2) extracting with organic solvent, separating the organic phase, drying with desiccant, and vacuum recovering to dry to obtain the product; (3) dissolving the product with eluting agent of mixed solution of hydrocarbon solvent and chlorine-containing solvent, eluting with alumina as filler of medium-pressure chromatography column, and collecting the fraction in a sectional manner; (4) mixing fractions with the Mezlocillin acid content of no smaller than 80%, vacuum concentrating, dissolving into ethanol, and basifying with base to separate precipitate; and (5) re-crystallizing the precipitate with ethanol, and freeze drying to obtain the high-purity Mezlocillin sodium.

Description

technical field [0001] The present invention relates to a method for preparing high-purity azlocillin sodium by continuous medium-pressure column chromatography, and also relates to a method for preparing azlocillin sodium powder injection from high-purity azlocillin sodium prepared by the method and a preparation method thereof, belonging to field of medical technology. Background technique [0002] Azlocillin is a penicillin antibiotic, which is effective against aerobic Gram-positive cocci such as Streptococcus pneumoniae, hemolytic Streptococcus, non-penicillinase-producing Staphylococcus, Enterococcus faecalis, Escherichia coli, Proteus mirabilis, Salmonella Non-β-lactamase-producing strains of aerobic Gram-negative bacteria such as Bacteria spp., Haemophilus influenzae, and Neisseria gonorrhoeae and Helicobacter pylori have good antibacterial activity. Azlocillin exerts a bactericidal effect by inhibiting the synthesis of bacterial cell walls, and can rapidly dissolve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D499/68A61K31/341A61K9/14A61P31/04
Inventor 邱民
Owner 海南华旗药业销售有限公司
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