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Method for analyzing content of acetyl bromide in cefuroxime axetil

A technology of cefuroxime axetil and an analysis method, applied in the field of analysis and detection, can solve the problems of inability to directly measure the content of cefuroxime axetil acetyl bromide, the influence of drug safety, etc., and achieves the advantages of short reaction time, reduced pollution and simple operation. Effect

Active Publication Date: 2022-04-15
SHANDONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, in the synthesis process of cefuroxime axetil, 1-acetoxy-1-bromoethane is generally used as a solvent, and acetyl bromide genotoxic impurities will be produced during the reaction decomposition process, which will affect the safety of the drug.
[0003] However, acetyl bromide is a highly active substance, which can be violently decomposed when encountering water and alcohol, and can react rapidly with nucleophilic substances. The liquid-mass method cannot directly determine the content of acetyl bromide in cefuroxime axetil

Method used

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  • Method for analyzing content of acetyl bromide in cefuroxime axetil
  • Method for analyzing content of acetyl bromide in cefuroxime axetil
  • Method for analyzing content of acetyl bromide in cefuroxime axetil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Linear, linear range analysis:

[0052] Proceed as follows:

[0053] Accurately measure an appropriate amount of acetyl bromide derivative solution of 75ng / ml, and dilute with acetonitrile to obtain linear solutions of 2.25ng / ml, 3.75g / ml, 7.5ng / ml, 11.25ng / ml, and 15ng / ml; , and then analyze the linear solution in turn, and draw a regression curve with the concentration of each linear solution versus the peak area.

[0054] Results Discussion:

[0055] Acetyl bromide standard curve as figure 1 As shown, Y=1.02e 6 X+1.44e 5 , r=0.9999; there is a linear relationship between the concentration of 2.26ng / ml~15.07ng / ml (corresponding to the limit concentration of 30%~200%), and the linear correlation coefficient r=0.9999.

Embodiment 2

[0057] Precision Analysis:

[0058] Proceed as follows:

[0059] (1) Blank test solution: Take about 10 mg of cefuroxime axetil, weigh it accurately, put it in a 5 ml sample preparation bottle, add 200 μl of 1 μg / ml 2,4-dinitrophenylhydrazine solution, vortex to dissolve, and derivatize After reacting for 1 h, add 1800 μl of acetonitrile, shake well, and obtain. Prepare 3 copies in the same way.

[0060](2) 100% standard-added test solution: Take about 10 mg of cefuroxime axetil, weigh it accurately, put it in a 5ml sample bottle, add 200 μl, 75ng of 1 μg / ml 2,4-dinitrophenylhydrazine solution successively 200 μl of reference substance derivatization solution per ml, vortex to dissolve, after 1 hour of derivatization reaction, add 1600 μl of acetonitrile, shake well, and obtain. Prepare 6 copies in the same way.

[0061] Results Discussion:

[0062] The precision inspection results of acetyl bromide are shown in Table 1 respectively.

[0063] Table 1 Results of precision...

Embodiment 3

[0066] Accuracy analysis:

[0067] Proceed as follows:

[0068] (1) Blank test solution: Take about 10 mg of cefuroxime axetil, weigh it accurately, put it in a 5 ml sample preparation bottle, add 200 μl of 1 μg / ml 2,4-dinitrophenylhydrazine solution, vortex to dissolve, and derivatize After reacting for 1 h, add 1800 μl of acetonitrile, shake well, and obtain. Prepare 3 copies in the same way.

[0069] (2) 50% standard-added test solution: Take about 10 mg of cefuroxime axetil, weigh it accurately, put it in a 5 ml sample preparation bottle, add 200 μl of 1 μg / ml 2,4-dinitrophenylhydrazine solution, 75ng / ml reference substance derivatization solution 100 μl, vortex to dissolve, after 1 hour of derivatization reaction, add 1700 μl of acetonitrile, shake well, and obtain. Prepare 3 copies in the same way.

[0070] (3) 100% standard-added test solution: Take about 10 mg of cefuroxime axetil, weigh it accurately, put it in a 5 ml sample preparation bottle, add 200 μ l of 1 μ...

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Abstract

The invention relates to the technical field of analysis and detection, in particular to a method for analyzing the content of acetyl bromide in cefuroxime axetil. According to the analysis method, the content of acetyl bromide in cefuroxime axetil is measured by using a triple four-stage liquid chromatograph-mass spectrometer, acetyl bromide is used as a reference substance, 2, 4-dinitrophenylhydrazine is used as a derivatization reagent, and the content of acetyl bromide in cefuroxime axetil is analyzed by using a standard curve method. According to the analysis method disclosed by the invention, the problems that acetyl bromide is extremely active, easy to hydrolyze and difficult to measure are solved through a pre-column derivatization method, and the detection method is efficient and accurate.

Description

technical field [0001] The invention relates to the technical field of analysis and detection, in particular to an analysis method for the content of acetyl bromide in cefuroxime axetil. Background technique [0002] Cefuroxime axetil is a second-generation cephalosporin with strong fat solubility. Oral administration by a patient can hydrolyze in the patient's body and release cefuroxime. Cefuroxime has a good antibacterial effect, and has a good effect in the treatment of mild and moderate respiratory tract infections, skin and soft tissue infections, genitourinary system infections and gonorrhea caused by sensitive bacteria. At present, 1-acetoxy-1-bromoethane is generally used as a solvent in the synthesis process of cefuroxime axetil, and acetyl bromide genotoxic impurities will be produced during the reaction decomposition process, which will affect the safety of the drug. [0003] However, acetyl bromide is a highly active substance, which can be violently decompose...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/86
Inventor 徐东王福芳王方
Owner SHANDONG UNIV
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