Method for detecting content of 3,5-substituted oxaolidones compound

A detection method, the technology of oxazolidinone, which is applied in the field of content detection of antibacterial drugs, can solve the problems of no compound detection method, poor solubility of the mobile phase, and the main component cannot be detected, etc., to achieve industrial production and The detection operation is convenient, the specificity is strong, and the effect of saving reagents

Active Publication Date: 2007-08-22
广东金城金素制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the structure is similar, if the above known methods are used to measure 3,5-substituted oxazolidinone compounds, the solubility of the mobile phase is not good, and each component cannot be effectively separated, and the main component cannot be detected, and it takes a long time
Since the 3,5-substituted oxazolidinone compound is a brand-new class of compounds, there is no detection method for this compound

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] Determination of detection wavelength

[0079] Sample (S)-[N-3-(3′-fluoro-4′-(4″-phenylpiperazinyl))phenyl-2-oxo-5-oxazolidinyl]methylacetamide The mobile phase was configured to a concentration of 5ug / ml, and scanned with ultraviolet light. As can be seen from the ultraviolet scanning spectrum, the maximum absorption wavelength of the compound was 257nm, so 257nm was selected as the detection wavelength for content determination.

Embodiment 2

[0081] (S)-[N-3-(3′-fluoro-4′-(4″-phenylpiperazinyl))phenyl-2-oxo-5-oxazolidinyl]methylacetamide in different Retention behavior in reversed-phase packed columns.

[0082] With acetonitrile-water (70:30) as the mobile phase, the flow rate is 1.0ml / ml. The injection volume is 20ul, the chromatogram is recorded at 257nm, and the chromatographic behavior in different reversed-phase C18 packed columns is investigated. The results are shown in Table 1 .

[0083] Table 1 Retention behavior in different ODS columns

[0084] Column packing and specification

[0085] It can be seen from Table 1 that all existing C18 brands can be used in (S)-[N-3-(3'-fluoro-4'-(4"-phenylpiperazinyl))phenyl-2- Oxo-5-oxazolidinyl] methyl acetamide and the content determination of preparation.Select Diamonsil ODS (200 * 4.6mm, 5um) to be chromatographic column, examine column temperature 20,30,40,50 ℃ respectively, the result shows Both (S)-[N-3-(3'-fluoro-4'-(4"-phenylpiperazinyl))phenyl-2-o...

Embodiment 3

[0087] Chromatographic conditions and system suitability test: use octadecylsilane bonded silica gel as filler, acetonitrile-water (75:25) as mobile phase; detection wavelength is 257nm, and the number of theoretical plates is according to (S)-[N- The peak value of 3-(3'-fluoro-4'-(4"-phenylpiperazinyl))phenyl-2-oxo-5-oxazolidinyl]methylacetamide should not be lower than 2500.

[0088] Preparation of reference solution: take (S)-[N-3-(3'-fluoro-4'-(4"-phenylpiperazinyl))phenyl-2-oxo which was dried at 105°C to constant weight -5-Oxazolidinyl]methylacetamide reference substance, accurately weighed, dissolved in mobile phase and diluted to a solution of 100ug / ml. Shake well to get ready.

[0089] Preparation of the test solution: Accurately weigh (S)-[N-3-(3′-fluoro-4′-(4″-phenylpiperazinyl))phenyl-2-oxo-5-oxo An appropriate amount of oxazolidinyl]methylacetamide is dissolved in the mobile phase and diluted to a solution of 100ug / ml, shaken well, and obtained.

[0090] Determi...

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Abstract

The invention provides a content testing method of 3, 5-replacing oxazolidone compound, which uses high-efficient liquid-phase chromatogram containing ultraviolet detector to test. Testing wavelength of the ultraviolet detector is 200-400nm. The fixed phase of high-efficient liquid-phase chromatogram is reverse phase pole and mobile of it is intermixture of water and polar organic solution. The method is characterized that sample solvency has high speed and efficiency, components in analyzed sample are separated thoroughly, preparation of corresponding regent is simple, analyzing method is stable and adaptability is strong.

Description

technical field [0001] The invention provides a method for detecting the content of 3,5-substituted oxazolidinone compounds using a high performance liquid phase method. In addition, the invention also provides content detection of antibacterial drugs with 3,5-substituted oxazolidinone compounds as active ingredients. Background technique [0002] In recent years, various types of antibiotics have been continuously developed and published, so that there are many targeted drugs for the treatment of bacterial infection diseases. While affirming their positive effects, it can also be seen that a large number of drug-resistant bacteria against antibacterial agents are also developing rapidly. After exposure to antimicrobial drugs, mutations mediated by plasmids or chromosomes can acquire drug resistance, which brings new difficulties to clinical treatment. As early as 1978, DuPont disclosed in the US4128654 patent that 5-halomethyl-3-aryl oxazolidinones had antibacterial activi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N33/15
Inventor 王莹朱锦刘劲松鲁韬
Owner 广东金城金素制药有限公司
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