Determination of Oxolinic Acid Residues in Gilthead Seabream ( Sparus aurata) Muscle Tissue and Plasma by High-Performance Liquid Chromatography.

Autor: Tyrpenou, A. E., Rigos, G.
Zdroj: Chromatographia; Dec2004, Vol. 60 Issue 11/12, p657-661, 5p
Abstrakt: 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. [ABSTRACT FROM AUTHOR]
Databáze: Complementary Index