Method for assaying 3,5-substituted oxazolidones compound content

A technology of oxazolidinone and determination method, which is applied in the direction of material analysis by observing the influence on chemical indicators, testing of pharmaceutical preparations, and analysis by making materials undergo chemical reactions, etc.

Inactive Publication Date: 2007-08-22
SICHUAN BEILIKE BIOTECH LIABILITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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There is currently no method for the content determi...

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  • Method for assaying 3,5-substituted oxazolidones compound content

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Experimental program
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Embodiment 1

[0099] The instrument model used in the potentiometric titration method is an automatic potentiometric titrator ZDJ-4A, and the manufacturer is Shanghai Silong Scientific Instrument Co., Ltd.

[0100] The sample test solution and titration solution used in the potentiometric titration method are the same as the non-aqueous titration method, but the judgment of the titration end point is automatically judged by the automatic potentiometric titrator, which reduces the error of human observation with the naked eye.

[0101] The specific method is: record the volume V consumed by the titrant and the reading mV of the potentiometer respectively, and calculate ΔE / ΔV. Take ΔE / ΔV as the ordinate and ΔV as the abscissa, as shown in Figure 1. The volume V at the highest peak of the graph is the volume of perchloric acid titrant consumed at the end of the titration.

[0102]Weigh (S)-[N-3-(3′-fluoro-4′-(4″-phenylpiperazinyl))phenyl-2-oxo-5-oxazolidinyl]methylacetamide Add glacial a...

Embodiment 2

[0107] Reagents: acetic anhydride, glacial acetic acid, formic acid, and crystal violet are of analytical grade.

[0108] Test solution: perchloric acid titration solution (0.1mol / L).

[0109] Preparation of crystal violet indicator solution: Take 0.5 g of crystal violet, add 100 ml of glacial acetic acid to dissolve it, and obtain it.

[0110] Preparation of perchloric acid titration solution (0.1mol / L): Take 750ml of anhydrous glacial acetic acid (calculated according to water content, add 5.22ml of acetic anhydride per 1g of water), add 8.5ml of perchloric acid (70-72%), shake Evenly, slowly add 23ml of acetic anhydride dropwise at room temperature, shake while adding, shake evenly after adding, let it cool, add an appropriate amount of anhydrous glacial acetic acid to make 1000ml, shake well, and let stand for 24 hours.

[0111] Accurately weigh compound 1: (S)-[N-3-(3′-fluoro-4′-(4″-phenylpiperazinyl))phenyl-2-oxo-5-oxazolidinyl] Add 50ml of glacial acetic acid to d...

Embodiment 3

[0115] Accurately weigh compound 1: (S)-[N-3-(3′-fluoro-4′-(4″-phenylpiperazinyl))phenyl-2-oxo-5-oxazolidinyl] Add 5ml of formic acid to dissolve 0.2g of methylacetamide, add 45ml of acetic anhydride, shake well, add 2 drops of crystal violet indicator solution, and titrate with perchloric acid titration solution (0.1mol / L) until the solution becomes blue-green, which is the titration Equivalent point. The titration result is corrected by the blank test, and the sample content is calculated. The results are shown in Table 3.

[0116] Table 3 (S)-[N-3-(3′-fluoro-4′-(4″-phenylpiperazinyl))phenyl-2-oxo-5-oxazolidinyl]methylacetamide Assay results

[0117] sample

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Abstract

The present invention provides a method for measuring 3, 5-substituted oxazolidone compound content, it is non-water detection method and includes: dissolving the sample by adding acid; adding crystal violet instruction liquid to the dissolved solution; titrating perchloric acid titrating solution to the solution till the solution becomes blue-green; and calculating the content of the sample. The method is convenient in the operation for the content measurement for chemical material medicine and content measurement for comparison sample, has accurate measuring result, and is simple in execution.

Description

technical field [0001] The invention provides a method for determining the content of 3,5-substituted oxazolidinone compounds, which is a non-aqueous titration method. The method is easy to operate in the content determination of chemical raw materials and reference substances. The result is accurate and easy to operate. Background technique [0002] Antimicrobial resistance is a major problem facing the world today. Since the 1980s, multidrug-resistant gram-positive bacteria have become the main pathogens of hospital-acquired pneumonia. At present, the treatment of Gram-positive bacterial infections is mostly caused by drug-resistant bacteria, so that there are very few therapeutic drugs available for clinical use, which has become a major clinical challenge. Staphylococci can acquire multidrug resistance, especially in nosocomial infections, but also in community-acquired infections. The drug resistance mechanism of pathogenic bacteria is also constantly evolving. Repor...

Claims

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Application Information

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IPC IPC(8): G01N21/79G01N33/15
Inventor 王莹朱锦刘劲松鲁韬
Owner SICHUAN BEILIKE BIOTECH LIABILITY
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