Determination of quinolone antimicrobial agents in strongly overlapped peaks from capillary electrophoresis using multivariate calibration methods

This paper describes a new procedure for the determination of quinolones ciprofloxacin and sarafloxacin in chicken muscle samples. It is based on a previously developed capillary zone electrophoresis (CZE) separation, in which all the quinolones regulated by EU Council Regulation number 2377/90 could be separated. However, as ciprofloxacin and sarafloxacin coelute in the CZE run and they have strongly overlapped spectra, separation between them is not possible. To overcome this problem, we have used a multivariate calibration procedure (partial least square regression (PLS-2)), applied to the spectra obtained at the maximum of the electrophoretic peaks, by using a diode array detector. The method has been validated by a combination of pure standards and fortified blank chicken muscle extracts. The recoveries obtained in the validation set were 101 +/- 6 and 93 +/- 6% for sarafloxacin and ciprofloxacin, respectively. The method has been also applied to chicken muscle samples, fortified at concentration levels between 100 and 350 mug kg(-), corresponding to values near the maximum residue level (MRL) regulated by the European Community. (C) 2003 Elsevier B.V. All rights reserved.