Determination of ibuprofen and tetrazepam in human urine by micellar electrokinetic capillary chromatography |
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Authors: | J J Berzas Nevado J Rodríguez Flores G Castañeda Peñalvo R M Rodríguez Dorado |
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Institution: | (1) Departamento de Química Analítica y Tecnología de Alimentos, Universidad de Castilla-La Mancha, 13071 Ciudad Real, Spain |
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Abstract: | A new micellar electrokinetic capillary chromatography method (MEKC) is proposed for the determination of ibuprofen and tetrazepam
in human urine samples over a concentration range of therapeutic interest. A fused silica capillary (60 cm × 75 μm) is used.
Ibuprofen and tetrazepam are detected via UV detection at 220 and 228 nm, respectively. Separation is performed at 25 °C and
at a separation voltage of 30 kV, with 15 mM borate buffer (pH 10.2) containing 40 mM sodium dodecylsulfate as the electrolyte
solution. Under these conditions the analytes were separated in <11 min. Sulfamethazine is used as an internal standard. Prior
to determination, the samples are purified and enriched by means of an extraction–preconcentration step with a preconditioned
C18 cartridge and by eluting the compounds with methanol. Good linearity, accuracy, precision, robustness and solution stability
were achieved for the technique. Detection limits of 200 μg L−1 for ibuprofen and 300 μg L−1 for tetrazepam were obtained. These analytes were then determined in real urine using the technique. |
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Keywords: | Ibuprofen Tetrazepam Capillary electrophoresis Robustness Urine |
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