DEVELOPMENT OF EXTRACTION PROCEDURE FOR ANALYSIS OF SEDATIVES AND beta-BLOCKERS IN SWINE KIDNEY

作者：de Oliveira Lenise G^*; Kurz Marcia H S; Goncalves Fabio F; Barreto Fabiano; Ruebensam Gabriel; Hoff Rodrigo

来源：Quimica Nova, 2014, 37(8): 1342-1350.

DOI：10.5935/0100-4042.20140185

• sedatives
• beta-blockers
• swine kidney

A procedure was developed for determination of 5 sedatives and 14 beta-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 (R) 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.

• 出版日期2014