A simple and rapid LC-MS/MS method for the determination of amphenicols in Nile tilapia

A quantitative method for analysis of amphenicols (chloramphenicol - CAP, thiamphenicol - TAP and florfenicol - FF) in Nile tilapia using LC-MS/MS is described. A simple sample preparation procedure was optimized using a Plackett-Burman design. The method was validated in accordance with Decision 2002/657/EC. Repeatability and reproducibility were less than 10.7% and 16%, respectively, for all compounds. Recoveries varied from 79.8% to 92.0%. CCα was 0.019, 54.81 and 54.93 μg.kg−1 for CAP, FF and TAP, respectively. CCβ was 0.068, 64.88 and 58.91 μg.kg−1 for CAP, FF and TAP, respectively. Limits of quantification (LOQ) were 12.5 μg.kg−1 for FF and TAP and 0.15 μg.kg−1 for CAP. Nile tilapia fillets (n = 32) analyzed did not contain chloramphenicol. Thiamphenicol was detected in one sample (3.1%) and florfenicol was detected in every sample, all of them at concentrations below the maximum residue limit.