Ceftazidime pentahydrate purifying method

A ceftazidime and purification method technology, which is applied in the field of ceftazime pentahydrate, can solve the problems of low recovery rate and failure to obtain ceftazidime pentahydrate crystals, etc., and achieve the effects of low cost, simple operation and high yield

Active Publication Date: 2006-05-24
GUANGZHOU BAIYUNSHAN PHARM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method is helpful to improve product purity and reduce polymer content, for ceftazidime preparations with high polymer content and poor color, according to this method, high-quality ceftazidime pentahydrate crystals still cannot be obtained
Simultaneously, this method first dissolves material in the higher system of pH, causes ceftazidime to degrade to some extent, reduces like this recovery rate

Method used

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  • Ceftazidime pentahydrate purifying method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] For unqualified ceftazime pentahydrate, the content of ceftazime determined by high performance liquid chromatography is 90.1wt.%, and the content of polymer determined by illuminating column chromatography is 8.5wt.%.

[0022] Suspend 20.0 g of the unqualified ceftazidime pentahydrate in 100 ml of water, cool to 0-5° C. in an ice-water bath, and add 36 wt.% concentrated hydrochloric acid dropwise while stirring until the material dissolves to obtain an aqueous solution of ceftazidime. Under stirring condition, in the ceftazidime aqueous solution, dropwise add 2N NaOH solution, adjust pH to 2.5, separate out off-white precipitate, filter off precipitate (precipitate wet weight 1.99g, HPLC detection contains ceftazidime 0.25g), obtain filtrate. Then, the resulting filtrate was heated up to 5-10°C in an ice-water bath, and 2N NaOH solution was added dropwise with stirring to make the pH 4.0, ceftazidime pentahydrate crystals were precipitated, and the temperature was adjus...

Embodiment 2

[0024] 20.0 g of the unqualified ceftazime pentahydrate of Example 1 was suspended in 100 ml of water, cooled to 0-5° C. with an ice-water bath, and 99 wt.% acetic acid was added dropwise while stirring until the material was dissolved to obtain a clarified aqueous solution of ceftazime. Then, 0.5 g of activated carbon was added to the obtained aqueous solution of ceftazidime, stirred and decolorized for 30 minutes, and then filtered to remove the activated carbon to obtain a filtrate. The resulting filtrate was kept in an ice-water bath to keep the temperature at 0-5°C. Under stirring, 22 wt.% ammonia water was added dropwise to adjust the pH to 2.0. An off-white precipitate was precipitated, and the precipitate was filtered off to obtain the filtrate. Then, the resulting filtrate was heated to 20-25°C in a water bath, and 22wt.% ammonia water was added dropwise under stirring, so that the pH was 4.2, and ceftazidime pentahydrate crystals were precipitated, and then the temper...

Embodiment 3

[0026] 20.0 g of the unqualified ceftazime pentahydrate of Example 1 was suspended in 30 ml of water, cooled to 0-5° C. with an ice-water bath, and 36 wt.% hydrochloric acid was added dropwise while stirring until the material was dissolved to obtain a clarified aqueous solution of ceftazime. Then, 0.5 g of activated carbon was added to the obtained aqueous solution of ceftazidime, stirred and decolorized for 30 minutes, and then filtered to remove the activated carbon to obtain a filtrate. The resulting filtrate was kept in an ice-water bath to keep the temperature at 0-5°C. Under stirring, 22 wt.% ammonia water was added dropwise to adjust the pH to 2.0. An off-white precipitate was precipitated, and the precipitate was filtered off to obtain the filtrate. Then, the resulting filtrate is heated to 20-25°C in a water bath, and 22wt.% ammonia water is added dropwise under stirring, so that the pH is 3.8, and ceftazidime pentahydrate crystals are precipitated, and then the tempe...

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Abstract

The method relates to a method for purifying ceftazidime, more concretely relating to a method for preparing high quality ceftazidime pentahydrate by impure, high-polymer impurity content ceftazidime through crystallization. It prepares impure, high-polymer impurity content ceftazidime pentahydrate, ceftazidime Hclú¼ceftazidime hydrobromide or ceftazidime overdue or recovered from the market, into a ceftazidime water solution, then regulates the pH value of the ceftazidime water solution to 1.5-2.5 by alkali or acid, here the impurity ceftazidime polymer is separated out with a little ceftazidime, and the separated-out matter is filtered, and the pH value of the filtrate is regulated to 3.5-4.8 by alkali so that the ceftazidime pentahydrate crystals are separated out. The method is simple and convenient to operate, low-cost, good-safety and high-yield. The obtained ceftazidime pentahydrate crystals are high purity and the polymer is low-content, reaching pharmacopoeia specified requirements.

Description

technical field [0001] The present invention relates to a method for purifying ceftazime, in particular to a method for preparing high-quality ceftazime pentahydrate from impure ceftazime containing polymer impurities through crystallization. Background technique [0002] Ceftazidime pentahydrate is a cephalosporin widely used clinically, and its structural formula is as follows: [0003] [0004] In order to ensure the safety of human medicine, the National Pharmacopoeia stipulates that for ceftazidime antibiotics, the content of ceftazidime pentahydrate is not less than 95%, the content of polymer is not more than 0.3%, and its color is not higher than No. 6 color. During storage, ceftazidime antibiotics tend to degrade and polymerize, especially when subjected to high temperature (>50°C), to form polymers such as ceftazidime dimers, trimers and polymers, which lead to the formation of active ingredients of the drug. The content is reduced, the color is strengthened...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/56
Inventor 冯胜昔黄伟东黄建军刘学斌刘晓红李葵英
Owner GUANGZHOU BAIYUNSHAN PHARM CO LTD
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