Abstract
A high-performance liquid chromatographic method for the determination of oxolinic acid (OA) residues in muscle tissue and plasma of the cultured fish gilthead seabream (Sparus aurata L.), is described. OA was extracted with ethyl acetate and after centrifugation the combined extracts were evaporated. To the remaining residue 1 mL of the mobile phase was added and the extract was partitioned with n-pentane which then was rejected by aspiration. OA was chromatographed on a Zorbax®SB-C18 column at 50oC and detected by fluorescence detection at λex 327 nm and λem 369 nm. The mobile phase was a mixture of 0.1% trifluoroacetic acid (v/v) pH 2.0 and acetonitrile-methanol 3:2 (v/v) in a combination of 50:50 (v/v) and a flow rate of 1.0 mL min−1, delivered isocratically. Method mean recovery (R%) achieved was 73.7 ± 4.4% (mean ± SD) for blank fortified samples (n=4) range at 50, 100 and 200 μg kg−1 with a RSD=3.3%. The limit of detection (LOD) was 2.0 μg kg−1 oxolinic acid in muscle tissue and plasma and the limit of quantification (LOQ) was 5.0 μg kg−1. The method is fast and suitable to be used with safety and accuracy for the control of OA residues in cultured seabreams and a trained analyst could carry out ready for chromatography more than 50 samples per working day.
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References
Drlica K, Coughlin S (1989) Pharmacol Ther 44: 107–122
EMEA (2000) Oxolinic Acid. Committee of the Veterinary Medicinal Products. The European Agency for the Evaluation of Medicinal Products. Summary Report (2). EMEA/MRL/753/00-Final
EMEA (1998) Oxolinic Acid. Committee of the Veterinary Medicinal Products.The European Agency for the Evaluation of Medicinal Products. Summary Report (1). EMEA/MRL/501/98-Final
Ledo A, Dopazo CP, Romalde JL, Toranzo AE, Barja JL (1987) Bull of the Eur Assoc Fish Pathol 7: 20–22
COMMISSION REGULATION (EC) No 739/2003 of 28 April 2003 amending Annex I to Council Regulation (EEC) No 2377/90 laying down a Community procedure for the establishment of maximum residue limits of veterinary medicinal products in foodstuffs of animal origin. Official Journal of the European Union L 106: 9–10
Rogstad A, Hormazabal V, Yndestad M (1989) J Liq Chromatogr 12: 3073–3086
Hustvedt SO, Salte R, Benjaminsen T (1989) J Chromatogr 494: 335–339
Samuelsen OB (1990) J Chromatogr 530: 452–457
Samuelsen OB (1994) J Chromatogr B: Biomed Appl 655: 311–314
Horie M, Saito K, Nose N, Nakazawa H (1995) SEZ 36: 62–78
Sved S, Larocque L, Weninger A, Schnurr M, Vas D (1991) In: EURORESIDUE Proceedings of conference on residues of veterinary drugs in foods, Haggsma N, Ruiter A (eds) Colophon. The Netherlands, pp. 335–360
Degroodt JM, Wyhowski De Bukanski B, Srebrnik S (1994) J Liq Chromatogr 17: 1785–1794
Hormazabal V, Yndestad M (2001) J Liq Chromatography Relat Technol 24: 109–115
Fish Farming Int (1998) 27: 16–19
Rigos G, Alexis M, Tyrpenou AE, Nengas I, Piper I, Troisi G (2002) J Fish Dis 25: 401–408
Rigos G, Nengas I, Alexis M, Tyrpenou AE, Troisi GM (2003) Aquaculture 224: 245–256
Tyrpenou AE, Kotzamanis YP, Alexis MN (2003) Aquaculture 220: 633–642
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Tyrpenou, A., Rigos, G. Determination of Oxolinic Acid Residues in Gilthead Seabream (Sparus aurata) Muscle Tissue and Plasma by High-Performance Liquid Chromatography. Chromatographia 60, 657–661 (2004). https://doi.org/10.1365/s10337-004-0445-z
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DOI: https://doi.org/10.1365/s10337-004-0445-z