<p>A new analytical approach was developed involving mag-netic solid-phase extraction (MSPE) and spectrofluorimetric determi-nation of propranolol (PRO) in biological fluids. A urine or plasma sample was prepared and adjusted to pH 3-4, then PRO was quickly</p>extracted using Fe3O4 magnetic nanoparticles (MNPs) modified by the surfactant sodium dodecyl sulfate (SDS) and determined applying spectrofluorimetry. Experimental conditions, such as the amount of MNPs and SDS, pH value, standing time, desorption solvent and maximal extraction volume have been adjusted to optimize the extraction process and to obtain analytical characteristics of the method. Linearity was observed in the analyte’s concentration range of 2-75 ng mL-1 for both urine and plasma samples. The correlation coefficients (r) were higher than 0.99. The method showed good precision and accuracy, with intra- and inter-assay precisions of less than 5.0% at all concentrations. Standard addition recovery tests were carried out, and the recoveries ranged from 79.4% to 90.4%. The limits of detection and quantification were 0.85 and 2.80 ng mL-1, respectively, for urine and 0.74 and 2.43 ng mL-1, respectively, for plasma. The method was applied to the determination of PRO in human urine and plasma samples.
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