scholarly journals Low-level Determination of 4-Hydrazino BenzoicAcid in Drug Substance by High Performance Liquid Chromatography/Mass Spectrometry

2010 ◽  
Vol 7 (2) ◽  
pp. 403-408 ◽  
Author(s):  
S. Harikrishna ◽  
K. Nagabhushana Reddy ◽  
Y. Suresh ◽  
M. Ramakrishna ◽  
M. Sarat ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Benzoic Acid ◽  
High Performance ◽  
Liquid Chromatography Mass Spectrometry ◽  
Monitoring Methods ◽  
Drug Substances ◽  
Ppm Level

HPLC/MS single ion monitoring methods have been evaluated for the determination of trace levels of 4- hydrazino benzoic acid (4-HBA) in drug substances. These 4-HBA have been highlighted as potential genotoxins. HPLC/MS was found to be more promising and limits of quantification was 0.52 ppm. For one drug substances excellent recoveries of 104.6% were obtained at the 0.5 ppm level.

scholarly journals A HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY METHOD DEVELOPMENT FOR THE QUANTITATIVE DETERMINATION OF ENALAPRIL MALEATE FROM CACO-2 CELL MONOLAYERS

2018 ◽  
Vol 11 (7) ◽  
pp. 89
Author(s):  
Liliya Logoyda
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Formic Acid ◽  
High Performance ◽  
Liquid Chromatography Mass Spectrometry ◽  
Enalapril Maleate ◽  
Cell Monolayers ◽  
Chromatography Mass Spectrometry

Objective: A simple, rapid high-performance liquid chromatography-mass spectrometry (HPLC MS/MS) method was developed for the determination of enalapril maleate from confluent Caco-2 monolayers and aqueous solution.Methods: Chromatography was achieved on Discovery C18, 50×2.1 mm, 5 μm column. Samples were chromatographed in a gradient mode (eluent A [acetonitrile-water-formic acid, 5: 95:0.1 v/v] and eluent B [acetonitrile-formic acid, 100:0.1 v/v]). The initial content of the eluent B is 0%, which increases linearly by 1.0 min to 100% and 1.01 min returns to the initial 0%. The mobile phase was delivered at a flow rate of 0.4 ml/min into the mass spectrometer ESI chamber. The sample volume was 5 μl.Results: Under these conditions, enalapril maleate was eluted at 1.52 min. According to the Caco-2 test results, enalapril showed low permeability. It should be noted that the recovery value for enalapril is 100.62 %. Low in vitro permeability data for enalapril are in good agreement with the literature data.Conclusion: From results of the analysis, it can be concluded that developed method is simple and rapid for determination of enalapril maleate from confluent Caco-2 monolayers and aqueous solution. Acquired results demonstrate that proposed strategy can be effortlessly and advantageously applied for examination of enalapril from Caco-2 cell monolayers.

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