Development and validation of a capillary zone electrophoresis method for the determination of propranolol and N-desisopropylpropranolol in human urine |
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Authors: | Juan José Berzas Nevado Juana Rodríguez Flores Francisco Javier Guzmán Bernardo |
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Institution: | a Regional Institute for Applied Scientific Research, University of Castilla-La Mancha, Avenida de Camilo José Cela 10, 13071 Ciudad Real, Spain b Department of Analytical Chemistry and Food Technology, Faculty of Chemical Sciences, Avenida de Camilo José Cela 10, 13071 Ciudad Real, Spain c Department of Analytical Chemistry and Food Technology, Faculty of Environmental Sciences, Avenida de Carlos III s/n, 45071 Toledo, Spain |
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Abstract: | A simple, rapid and sensitive procedure using solid phase extraction and capillary zone electrophoresis for the determination of propranolol (a beta-blocker) and one of its metabolites, N-desisopropylpropranolol, has been developed and validated. The optimum separation of both analytes was obtained in a 37 cm × 75 μm fused silica capillary using 20 mmol/L phosphate buffer (pH 2.2) as electrolyte, at 25 kV and 30 °C, and hydrodynamic injection for 5 s. Prior to the electrophoretic separation, the samples were cleaned up and concentrated using a C18 cartridge and then, eluted with methanol, allowing a concentration factor of 30.Good results were obtained in terms of precision, accuracy and linearity. The limits of detection were 28 and 30 μg/L for N-desisopropylpropranolol and propranolol, respectively. Additionally, a robustness test of the method was carried out using the Plackett-Burman fractional factorial model with a matrix of 15 experiments.The presented method has been applied to the determination of both compounds in human urine. |
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Keywords: | Capillary zone electrophoresis Propanolol N-desisopropylpropanolol Ruggedness Urine determination |
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