Development and validation of a multiresidue method for the determination of antibiotic residues in crawfish using LCMS/MS

This study developed a rapid multi-class method for determining 29 antibiotic residues in crawfish using liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. A quick and affordable extraction method was employed, and sample preparation was performed using a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) technique. The extraction process involved adding acetonitrile to crawfish samples. The sample was homogenised with a solution of sodium citrate buffer and sodium EDTA, followed by a cleanup step. The method was validated according to European Union (EU) guidelines 2002/657/EC. The limit of quantitation (LOQ) for all antibiotics was 5 mu g/kg, except for flumequine and trimethoprim, which had LOQs of 2.5 mu g/kg. The LOQ for the tetracycline group was 25 mu g/kg, and for chloramphenicol, it was 0.015 mu g/kg. The average recoveries at different concentration levels varied between 60-120%. The precision, expressed as repeatability and reproducibility, was calculated to be less than 16%. Thirty crawfish samples collected from local Egyptian market were monitored for antibiotic residues. The results revealed contamination with antibiotics belonging to three different groups. Of the thirty samples, 27% were contaminated with ciprofloxacin and enrofloxacin, 17% with chlortetracycline and oxytetracycline, 7% with oxolinic acid, and 3% with sulphamethazine. The applicability of the developed method was proven through successful proficiency testing. The developed method met performance criteria and is suitable for monitoring these antibiotics in crawfish.