Latamoxef hydroxyl impurity preparation method

A technology of latamoxef hydroxy and oxyceph hydroxy, which is applied in the field of preparation of latamoxef hydroxy impurities, can solve the problems of few samples, poor impurity stability, and difficulty in obtaining pure samples, so as to achieve a large amount of sample acquisition and improve the overall quality level , the effect of high purity

Pending Publication Date: 2021-09-07
福安药业集团重庆博圣制药有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There is an impurity in Latamoxef Sodium, only the Chinese Institute for Food and Drug Control published the article "LC / MSn Rapid Analysis of Impurity Profile of Latamoxef Sodium Raw Materials" in China Antibiotic Impurities, Volume 44, Issue 7, July 2019 The results of liquid mass analysis of this impurity in Latamoxef sodium were mentioned. Due to the poor stability of this impurity, it is extremely difficult to obtain a sample with high purity by preparative chromatographic separation from the mother liquor, and it is limited by the sample loading capacity of the preparative chromatographic column and the content of the impurity in the mother liquor, although it takes a lot of time, only a very small sample can be obtained
Moreover, since the separation principle of preparative chromatography is that after the material liquid enters the chromatographic column, the components in it are respectively eluted by the filler and then eluted by the mobile phase. The disadvantage of this separation method is that the concentration of the obtained target product solution is generally below 1%. Enrichment by means of concentration or extraction can only be used for lyophilization, and due to the limited separation capacity of the preparative chromatographic column, the amount of sample loaded each time cannot be too much, so repeated separations are required, and the target product solution is combined for enrichment treatment
There is currently no search for a method that can be prepared in large quantities

Method used

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  • Latamoxef hydroxyl impurity preparation method
  • Latamoxef hydroxyl impurity preparation method
  • Latamoxef hydroxyl impurity preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 50 g of tap water and 20 g of crystalline latamoxef sodium into a 250 ml reaction bottle, stir to dissolve, add 2.1 g of sodium hydroxide / 50 g of tap water solution, and react at a temperature of 40° C. for 5 hours. Cool down to room temperature, pass the reaction solution through the DM-2 resin column, and control the temperature of the resin column jacket at 2-10°C. After feeding the liquid, wash it with purified water. The bottom effluent is monitored with a capillary tube until there is 254nm fluorescence color development, and then the effluent is collected. 45-50 grams, after freeze-drying at the highest drying temperature of 5°C, 5.3 g of a light yellow solid was obtained, with a yield of 32.1%.

Embodiment 2

[0037] Add 70 g of tap water and 20 g of crystalline latamoxef sodium into a 250 ml reaction bottle, stir to dissolve, add 2.6 g of sodium hydroxide / 50 g of tap water solution, and react at a temperature of 45° C. for 5 hours. Cool down to room temperature, pass the reaction solution through the DM-2 resin column, and control the temperature of the resin column jacket at 2-10°C. After feeding the liquid, wash it with purified water. The bottom effluent is monitored with a capillary tube until there is 254nm fluorescence color development, and then the effluent is collected. 45-50 g, after lyophilization at the highest drying temperature of 5°C, 5.1 g of light yellow solid was obtained, with a yield of 30.9%.

[0038] Preparation by preparative chromatography 1 only about 2 mg of sample can be obtained for each separation, but by this method for preparation, the concentration of the feed liquid after passing through the macroporous resin can reach 10%-20%, and the direct freeze-...

Embodiment 3

[0039] Example 3 Sample Characterization

[0040] The Latamoxef hydroxyl impurity prepared by embodiment 2 is carried out to proton nuclear magnetic spectrum analysis, and analysis proton spectrogram is as follows figure 1 shown.

[0041] The Latamoxef hydroxyl impurity prepared in embodiment 2 is carried out carbon nuclear magnetic spectrum analysis, and analysis carbon spectrogram is as follows figure 2 shown.

[0042] The Latamoxef hydroxyl impurity prepared by embodiment 2 is carried out to mass spectrometry, and the analysis mass spectrogram is as follows image 3 shown.

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Abstract

The invention belongs to the technical field of chemical medicine preparation, and particularly relates to a latamoxef hydroxyl impurity preparation method which comprises comprises the steps: mixing a latamoxef sodium aqueous solution and a sodium hydroxide aqueous solution, and carrying out a heat preservation reaction to obtain a; and then separating the a by using macroporous resin, and freeze-drying. The preparation method has the advantages of being simple and easy to operate, high in purity and large in sample obtaining amount. The prepared latamoxef hydroxyl impurity is convenient for quality research of latamoxef sodium, especially provides a large batch of impurity reference substances with uniform quality for quantifying the impurity content in latamoxef sodium by adopting an external standard method, is beneficial to improving the overall quality level of latamoxef sodium, and lays a foundation for the variety to reach the quality level of a reference preparation.

Description

technical field [0001] The invention belongs to the technical field of chemical medicine preparation, and in particular relates to a preparation method of latamoxef hydroxy impurity. Background technique [0002] Latamoxef sodium is a semi-synthetic oxycephem antibiotic. Its basic structure is close to that of cephamycins, only the S in the first position of the mother nucleus is replaced by O. This product has broad-spectrum and bactericidal effect, and its antibacterial effect is similar to that of the third-generation cephalosporins. The antibacterial spectrum is similar to that of cefotaxime. It has good antibacterial effect on a variety of Gram-negative bacteria, including Escherichia coli, Haemophilus influenzae, Klebsiella, Proteus, Enterobacter, Citrobacter, Serratia Chemicalbook, etc. Strong antibacterial activity; good antibacterial activity against anaerobic bacteria such as Bacteroides fragilis; antibacterial effect against Acinetobacter and Pseudomonas is wor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D505/06C07D505/20
CPCC07D505/06C07D505/20
Inventor 夏秦川洪荣川袁明华廖勇群付倩文杨敏谭超丁东
Owner 福安药业集团重庆博圣制药有限公司
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