RESUMO
A highly sensitive, rapid assay method has been developed and validated for the estimation of bicalutamide in mouse plasma using liquid chromatography coupled to tandem mass spectrometry with electrospray ionization in the negative-ion mode. The assay procedure involves extraction of bicalutamide and tolbutamide (internal standard, IS) from mouse plasma with a simple protein precipitation method. Chromatographic separation was achieved using an isocratic mobile phase (0.2% formic acid:acetonitrile, 35:65, v/v) at a flow rate of 0.5 mL/min on an Atlantis dC18 column (maintained at 40 ± 1°C) with a total run time of 3.0 min. The MS/MS ion transitions monitored were m/z 428.9 â 254.7 for bicalutamide and m/z 269.0 â 169.6 for IS. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. The lower limit of quantitation achieved was 1.04 ng/mL and the linearity range extended from 1.04 to 1877 ng/mL. The intra- and inter-day precisions were in the ranges of 0.49-4.68 and 2.62-4.15, respectively.
Assuntos
Anilidas/sangue , Cromatografia Líquida de Alta Pressão/métodos , Nitrilas/sangue , Espectrometria de Massas em Tandem/métodos , Compostos de Tosil/sangue , Anilidas/química , Anilidas/farmacocinética , Animais , Estabilidade de Medicamentos , Limite de Detecção , Modelos Lineares , Camundongos , Camundongos Endogâmicos BALB C , Nitrilas/química , Nitrilas/farmacocinética , Reprodutibilidade dos Testes , Espectrometria de Massas por Ionização por Electrospray/métodos , Compostos de Tosil/química , Compostos de Tosil/farmacocinéticaRESUMO
A highly sensitive, rapid assay method was developed and validated for the estimation of lorglumide in mouse plasma using liquid chromatography coupled to tandem mass spectrometry with electrospray ionization in positive-ion mode. The assay procedure involves extraction of lorglumide and phenacetin (internal standard, IS) from mouse plasma with simple protein precipitation. Chromatographic separation was achieved using an isocratic mobile (0.2% formic acid solution-acetonitrile, 20:80, v/v) at a flow-rate of 0.5 mL/min on an Atlantis dC18 column maintained at 40 °C with a total run time of 4.0 min. The MS/MS ion transitions monitored were 459.2 â 158.4 for lorglumide and 180.1 â 110.1 for IS. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. The lower limit of quantitation achieved was 0.42 ng/mL and the linearity range extended from 0.42 to 500 ng/mL. The intra- and inter-day precisions were in the ranges of 1.47-10.9 and 3.56-7.53, respectively.
