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.
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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 aceti...
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 disso...
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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