On-line coupling of solid-phase extraction and capillary electrophoresis for the determination of cefoperazone and ceftiofur in plasma

Autor: Gerhardus J. de Jong, Carme Aguilar, Marta Calull, F. W. Alexander Tempels, Francesc Borrull, Patricia Puig, Govert W. Somsen
Přispěvatelé: BioAnalytical Chemistry, AIMMS
Jazyk: angličtina
Rok vydání: 2007
Předmět:
Zdroj: Puig, P, Tempels, F W A, Borrull, F, Calull, M, Aguilar, C, Somsen, G W & de Jong, G J 2007, '
coupling of solid-phase extraction and capillary electrophoresis for the determination of cefoperazone and ceftiofur in plasma ', Journal of Chromatography B, vol. 856, no. 1-2, pp. 365-370 . https://doi.org/10.1016/j.jchromb.2007.05.030
Journal of Chromatography B, 856(1-2), 365-370. Elsevier
ISSN: 1873-376X
1570-0232
DOI: 10.1016/j.jchromb.2007.05.030
Popis: We present a method for determining two cephalosporins (cefoperazone and ceftiofur) in plasma by on-line solid-phase extraction (SPE)-capillary zone electrophoresis (CZE) with a T-split interface. Using this interface, a part of the SPE elution plug containing the cephalosporins is injected while the rest of the sample is flushed to waste. SPE was carried out using a C(18) micro-precolumn and the cephalosporins presented good retention properties with breakthrough volumes above 1 ml. Using a desorption volume of 426 nl of acetonitrile, recoveries were 75 and 90%, for cefoperazone and ceftiofur, respectively. The resulting elution volume was about 1.8 microl. A deproteinization step was included prior to SPE for the analysis of plasma samples with recoveries of 90 and 57% for cefoperazone and ceftiofur, respectively. With UV detection at 254 nm, linear relationships between the injected concentration and peak area was measured between 10 and 500 ng ml(-1) for standards, and 200 and 1500 ng ml(-1) for plasma samples. Intra-day (n=5) and inter-day (n=5) peak area repeatability were lower than 12% RSD. The detection limits obtained for spiked plasma (100 ng ml(-1) cefoperazone and ceftiofur) are sufficient for applying the method to pharmacokinetic studies.
Databáze: OpenAIRE