RESUMO
A method for determination of thyreostatic residues in animal tissues by matrix solid-phase dispersion (MSPD) and gas chromatography-mass spectrometry in selected ion detection mode was developed. Thyreostatic compounds in different matrices were extracted and purified by combination of MSPD and subsequent solid-phase extraction. Silica gel was selected as the solid support of both procedures and the conditions of the procedures were optimized. Thyreostats were derivatized with pentafluorobenzylbromide (PFBBr) in strong basic medium and then with N-methyl-N-(trimethylsilyl)-trifluoroacetamide (MSTFA), which can improve the yields of derivatization for thyreostats, the repeatability, and therefore the limits of detection (LOD) of thyreostats. The limits of detection reached 10 microg/kg (2-thiouracil, 6-methyl-2-thiouracil and 6-propyl-2-thiouracil), 20 microg/kg (6-phenyl-2-thiouracil) and 50 microg/kg (tapazole) with high recoveries (more than 70% for most of thyreostats) and relative standard deviations between 4.5% and 8.7%.
Assuntos
Antitireóideos/análise , Fluoracetatos , Acetamidas , Animais , Antitireóideos/isolamento & purificação , Fluorbenzenos , Cromatografia Gasosa-Espectrometria de Massas/métodos , Metimazol/isolamento & purificação , Metiltiouracila/isolamento & purificação , Propiltiouracila/isolamento & purificação , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Sílica Gel , Dióxido de Silício , Suínos , Tiouracila/isolamento & purificação , Compostos de TrimetilsililRESUMO
Capillary zone electrophoresis was optimized for the separation of thiouracil, methylthiouracil and propylthiouracil. Methylthiouracil could be determined in various types of urine (human, bovine, horse), either without any pretreatment or in ethyl acetate extracts, within 15 min. For identification, the simultaneous detection at three UV wavelengths (216, 245 and 278 nm) was advantageously used while for quantification the wavelength of the absorbance maximum at 278 nm was preferred. Under optimized conditions a linear response of the detector in the concentration range 0.1-100 ppm was obtained. On analysis of untreated urine, a detection limit of 0.5 ppm was found; for urine extracts the detection limit was 0.1 ppm. Univocal peak identification, based on absorption at three wavelength, was only possible above 2 ppm. Relative standard deviation for standard solutions of methylthiouracil, diluted in the background electrolyte, was 1%; for methylthiouracil in extracts dissolved in the background electrolyte it was 4.5%, and for methylthiouracil in untreated urine, 12.7%.
