Desenvolvimento de procedimento de extração para análise de sedativos e B-bloqueadores em rim suíno

AUTOR(ES)

Oliveira, Lenise G. de, Kurz, Marcia H. S., Gonçalves, Fábio F., Barreto, Fabiano, Rübensam, Gabriel, Hoff, Rodrigo

FONTE

Quím. Nova

DATA DE PUBLICAÇÃO

2014

RESUMO

A procedure was developed for determination of 5 sedatives and 14 β-blockers in swine kidney and subsequent analysis by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Three different procedures for extraction were tested, evaluated through recovery studies. The procedure using acetonitrile for extraction and cleanup with freezing at low temperature and dispersive solid phase extraction using 500 mg celite® 545 before the concentration step presented the better results. The dried samples were redissolved with methanol and analyzed using a LC-MS/MS system with electrospray ionization (ESI) operating in positive MRM mode. The recovery values for this procedure were in the 75-88% range. The robustness of the method was tested against small variations. The method was used to analyze carazolol, azaperone and azaperol in collaborative assay, obtaining results close to designed value.

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