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Determination of the glucocorticoid fluticasone propionate in plasma by automated solid-phase extraction and liquid chromatography–tandem mass spectrometry
Authors:Sheryl L Callejas  Robert A Biddlecombe  Anne E Jones  Karina B Joyce  Adrian I Pereira  Stephen Pleasance
Affiliation:Department of International Bioanalysis, Division of Bioanalysis and Drug Metabolism, GlaxoWellcome Research and Development, Park Road, Ware, Herts., SG12 0DP, UK
Abstract:A sensitive, robust and high throughput mass spectrometry based method is described for the determination of the glucocorticoid fluticasone propionate in plasma. The method employs solid-phase extraction in 96 well microtitre plate format which has been automated by means of a custom built Zymark robotic system. The extracts are analysed by liquid chromatography–tandem mass spectrometry using thermally and pneumatically assisted electrospray ionisation and selected reaction monitoring. The method is both accurate and precise with both intra- and inter-assay precision (C.V.) of less than <6%. The method provides a lower limit of quantification of 20 pg/ml from 0.5 ml of human plasma, sufficient to monitor systemic concentrations of inhaled fluticasone propionate at therapeutic doses.
Keywords:Fluticasone propionate   Glucocorticoid
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