In this study a new spectrofluorimetric method for the direct determination of metoprolol in human plasma is presented and discussed. It is based on the use of fluorescence excitation-emission matrices (EEMs) and second-order calibration performed with parallel factor analysis (PARAFAC) or alternating trilinear decomposition (ATLD). This methodology enables accurate and reliable discrimination of the analyte signal, even in the presence of unknown and uncalibrated fluorescent component(s), which is often referred to as the second-order advantage. No separation or sample pretreatment steps were required. Satisfactory results were obtained. Metoprolol recoveries in plasma were determined as 87+/-2% and 90+/-4% with PARAFAC and ATLD, respectively. All RSD values of intra- and interday assays were below 5%.
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