Journal
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
Volume 856, Issue 1-2, Pages 365-370Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.jchromb.2007.05.030
Keywords
solid-phase extraction; capillary electrophoresis; on-line; cephalosporins; plasma samples
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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 mu l. 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 254nm, linear relationships between the injected concentration and peak area was measured between 10 and 500ng 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. (C) 2007 Elsevier B.V. All rights reserved.
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