Quantitation of oxcarbazepine and its metabolites in human plasma by micellar electrokinetic chromatography |
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Authors: | Pucci Vincenzo Kenndler Ernst Raggi Maria Augusta |
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Institution: | Department of Pharmaceutical Sciences, University of Bologna, Via Belmeloro 6, 40126 Bologna, Italy. |
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Abstract: | A reliable micellar electrokinetic chromatographic method for the determination of oxcarbazepine and its two main metabolites, 10-hydroxycarbamazepine and 10,11-trans-dihydroxy-10,11-dihydroxycarbamazepine, in human plasma was developed. The separation and determination of the analytes was achieved using a system consisting of 60 mM SDS in phosphate buffer (30 mM, pH 8.0), to which 20% (v/v) methanol was added. Separation was carried out in an uncoated fused-silica capillary with a separation voltage of 25 kV and currents typically less than 40 microA. Spectrophotometric detection was at 205 nm. Isolation of oxcarbazepine and its metabolites from plasma was accomplished by a solid-phase extraction procedure. The mean extraction yield of the analytes from plasma was higher than 94%. The linear correlation coefficients were better than 0.994 for all analytes. The limit of detection was 0.05 microg/mL, the limit of quantitation 0.15 microg/mL. The repeatability for the spiked blank plasma samples was lower than 1.9% and the intermediate precision lower than 2.1%, both expressed as RSD%. The results obtained analysing real plasma samples from epileptic patients under therapy with Tolep were satisfactory in terms of precision, accuracy and detectability. |
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Keywords: | antiepileptic carbamazepine 10 11‐dihydro‐10‐oxo‐5H‐dibenz‐[b f]azepin‐5‐carboxamide 10 11‐dihydro‐10‐hydroxy‐carbamazepine trans‐10 11‐dihydro‐10 11‐dihydroxycarbamazepine solid‐phase extraction |
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