Measurement of tulobuterol in human plasma by capillary gas chromatography and selected ion monitoring detection

Abstract

A method is described for the quantification of tulobuterol in human plasma, based upon selective extraction and high resolution capillary gas chromatography-mass spectrometry. The mass spectrometric determination is based on selected ion monitoring of two fragment ions derived from the N,O-heptafluorobutyryl derivatives of tulobuterol and its internal standard, deschlorotulobuterol. The plasma work-up procedure consists of extraction of 1.0 ml alkalinised plasma with dichloromethane, back-extraction into an acidified aqueous phase, followed by a final extraction with dichloromethane after realkalinisation. The method gave interference-free and linear results. The between-assay variability is 4.7% CV at the 3.0 micrograms l-1 plasma concentration level. The assay permitted quantitative measurements down to 170 ng tulobuterol per litre of plasma and hence provided sufficient sensitivity for quantification of plasma levels after therapeutic doses.