PMID- 20496028 OWN - NLM STAT- MEDLINE DCOM- 20101008 LR - 20160512 IS - 1618-2650 (Electronic) IS - 1618-2642 (Linking) VI - 397 IP - 6 DP - 2010 Jul TI - Determination of fluoroquinolone residues in poultry muscle in Portugal. PG - 2615-21 LID - 10.1007/s00216-010-3819-0 [doi] AB - A total of 98 poultry samples, including chicken and turkey muscle, were analysed, using a sensitive and reliable analytical method based on liquid chromatography (LC) with spectrofluorimetric detection, for simultaneous determination of four fluoroquinolone (FQ) antibiotics, namely enrofloxacin (ENRO), ciprofloxacin (CIPRO), norfloxacin (NOR), and sarafloxacin (SARA). The method involved extraction with 0.15 mol L(-1) HCl and clean-up by solid-phase extraction using Oasis HLB cartridges. Chromatographic separation was carried out on a C(18) TSK gel column, in isocratic mode, with 0.025 mol L(-1) H(3)PO(4) solution, adjusted to pH 3.0 with tetrabutylammonium hydroxide-methanol (78:22) as mobile phase. Good linearity over the investigated concentration range was observed, with mean values of correlation coefficients higher than 0.9989 for all the analytes studied. The limits of quantification (LOQ), expressed as the lowest fortification level with acceptable precision were 15 microg kg(-1) for ENRO, CIPRO, and NOR, and 30 microg kg(-1) for SARA; these values are in compliance with requirements for monitoring of maximum residues levels (MRLs). Overall recoveries from spiked samples ranged from 80% to 92% with relative standard deviations (RSD) lower than 6.1%. Of the chicken and turkey samples analysed, 44.2% and 37.8%, respectively, were contaminated. The levels found in the analysed poultry samples, collected from markets of Oporto and Coimbra, located in the north and central zones of Portugal, respectively, were lower than 114.2 and 87.6 microg kg(-1) in chicken and turkey muscle samples, respectively. One positive chicken sample was contaminated with ENRO at levels higher than the MRL. FAU - Pena, A AU - Pena A AD - Group of Health Surveillance, CEF, Faculty of Pharmacy, University of Coimbra, Health Sciences Campus, Azinhaga de Santa Comba, 3000-548 Coimbra, Portugal. apena@ff.uc.pt FAU - Silva, L J G AU - Silva LJ FAU - Pereira, A AU - Pereira A FAU - Meisel, L AU - Meisel L FAU - Lino, C M AU - Lino CM LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20100522 PL - Germany TA - Anal Bioanal Chem JT - Analytical and bioanalytical chemistry JID - 101134327 RN - 0 (Anti-Bacterial Agents) RN - 0 (Fluoroquinolones) SB - IM MH - Animals MH - Anti-Bacterial Agents MH - Chromatography, Liquid/methods MH - Drug Residues/*analysis MH - Fluoroquinolones/*analysis MH - Food Contamination/*analysis MH - Limit of Detection MH - Muscles/chemistry MH - Portugal MH - *Poultry MH - Reproducibility of Results EDAT- 2010/05/25 06:00 MHDA- 2010/10/12 06:00 CRDT- 2010/05/25 06:00 PHST- 2010/03/31 00:00 [received] PHST- 2010/05/02 00:00 [accepted] PHST- 2010/04/22 00:00 [revised] PHST- 2010/05/25 06:00 [entrez] PHST- 2010/05/25 06:00 [pubmed] PHST- 2010/10/12 06:00 [medline] AID - 10.1007/s00216-010-3819-0 [doi] PST - ppublish SO - Anal Bioanal Chem. 2010 Jul;397(6):2615-21. doi: 10.1007/s00216-010-3819-0. Epub 2010 May 22.