ABSTRACT
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⯵g.kg-1 for CAP, FF and TAP, respectively. CCß was 0.068, 64.88 and 58.91⯵g.kg-1 for CAP, FF and TAP, respectively. Limits of quantification (LOQ) were 12.5⯵g.kg-1 for FF and TAP and 0.15⯵g.kg-1 for CAP. Nile tilapia fillets (nâ¯=â¯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.
Subject(s)
Chloramphenicol/analysis , Chromatography, Liquid/methods , Cichlids , Fish Products/analysis , Tandem Mass Spectrometry/methods , Thiamphenicol/analogs & derivatives , Thiamphenicol/analysis , Animals , Anti-Bacterial Agents/analysis , Limit of Detection , Reproducibility of ResultsABSTRACT
Bee products can be produced in an environment contaminated by pesticides that can be transported by honey bees to the hive and incorporated into the honey. Therefore, rapid and modern methods to determine pesticide residues in honey samples are essential to guarantee consumers' health. In this study, a simple multiresidue method for the quantification of 116 pesticides in honey is proposed. It involves the use of a modified QuEChERS procedure followed by UHPLC-MS/MS analysis. The method was validated according to the European Union SANCO/12571/2013 guidelines. Acceptable values were obtained for the following parameters: linearity, limit of detection (0.005mg/kg) and limit of quantification (0.010 and 0.025mg/kg), trueness (for the four tested levels the recovery assays values were between 70 and 120%), intermediate precision (RSD<20.0%) and measurement uncertainty tests (<50.0%). The validated method was applied for determination of 100 honey samples from five states of Brazil.
