RESUMO
The purpose of the study was to develop and validate a sensitive, selective and reproducible method for the estimation of Celecoxib in human plasma. During the development, ion competition phenomenon observed in electrospray ionization ion source of liquid chromatography mass spectrometer system and in order to overcome it, different approaches applied. The Celecoxib and Celecoxib D7 in plasma were extracted by liquid-liquid extraction and separated in less than 4.0 min on a reverse phase C18 column, using isocratic elution with a binary mobile phase in the ratio of 70:30 v/v (Acetonitrile: 0.1% Ammonia Solution). Mass spectrometer was used as detector to quantitate the analytes in positive ion mode, using Atmospheric Pressure Chemical Ionization mode. Since the method was developed to perform the pharmacokinetic end point study for United States and Europe market, the method was fully validated, complying Food and Drug Administration, European Medicines Agency guideline and recommendations of American Association of Pharmaceutical Scientists white papers.
Assuntos
Celecoxib/sangue , Plasma/química , Cromatografia Líquida/métodos , Europa (Continente) , Humanos , Indicadores e Reagentes/química , Preparações Farmacêuticas/sangue , Reprodutibilidade dos Testes , Espectrometria de Massas por Ionização por Electrospray/métodos , Espectrometria de Massas em Tandem/métodos , Equivalência TerapêuticaRESUMO
A convenient synthesis of oximes of steroidal chalcones (4a-4j) was performed and structural assignment of the products was confirmed on the basis of IR, (1)HNMR, (13)C NMR, MS and analytical data. The synthesized compounds were screened for in vitro antioxidant activity by using DPPH method and in vitro antimicrobial activity against different bacterial and fungal strains by agar diffusion method. The activity of the tested compounds against each microbe varied due to structural differences between them. Presence and position of different substituents on the benzene ring of the chalconyl pendent had a marked effect on the activity of the compounds. From the results it can be inferred that the compounds 4a-j showed significant antioxidant activity and antimicrobial activity against all microbial strains used for testing.
