Determination of quinolones in chicken muscle by Liquid Chromatography with diode array detector (LC-DAD) using QuEChERS as treatment technique

Abstract

A quick, easy, cheap, effective, rugged and safe method, using QuEChERS extraction followed by high-performance liquid chromatography with DAD detection (HPLC-DAD), has been developed for the determination of quinolones (norfloxacine, ciprofloxacine, danofloxacine, difloxacine, sarafloxacine and flumequine) in chicken muscle. Chromatographic separation was achieved using acidified water (acetic
acid 0.1 M, pH = 2.8) and methanol (85:15) as mobile phase with C8 column (150 mm x 4,6 mm i.d., 5 μm particle size). All analytes eluted before 18 minutes, at a flow of 1 mL min-1, at two wavelengths for detection, 250 and 280nm, respectively. The sample treatment consisted of extraction and cleanup using the QuEChERS methodology, for which different variables were optimized, showing high efficiency without the presence of interferences in the chromatographic separation. The method presented adequate linearity (r2>0.90) and recoveries between 70 and 110 %. The limits of detection (S/N=3) were lower than the maximum residue limits (MRL) established for quinolones, and the intra- and inter-day variation coefficients (n=3) at three concentration levels, were between 3.8 and 10.9 %. A total of 36 samples, obtained in Tegucigalpa and Comayagüela in Honduras, were analyzed by the proposed method, and traces of flumequine were found in two of them.