Open AccessDEVELOPMENT OF EXTRACTION PROCEDURE FOR ANALYSIS OF SEDATIVES AND β-BLOCKERS IN SWINE KIDNEY
Author(s) -
Lenise Guimarães de Oliveira,
Márcia Helena Scherer Kurz,
Fábio Ferreira Gonçalves,
Fabiano Barreto,
Gabriel Rübensam,
Rodrigo Barcellos Hoff
Publication year - 2014
Publication title -
química nova
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.214
H-Index - 73
eISSN - 1678-7064
pISSN - 0100-4042
DOI - 10.5935/0100-4042.20140185
Subject(s) - extraction (chemistry) , medicine , chromatography , chemistry
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