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 for CAP, FF and TAP, respectively. CCβ was 0.068, 64.88 and 58.91 μg.kg for CAP, FF and TAP, respectively. Limits of quantification (LOQ) were 12.5 μg.kg for FF and TAP and 0.15 μg.kg 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.
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