Multiclass method for detecting 41 antibiotic residues in bovine liver, muscle, and milk using LC-Q-Orbitrap-HRMS

Abstract

This study developed and validated an analytical method for the simultaneous identification and quantification of 41 veterinary antibiotic drugs from 9 different classes, including sulfonamides, quinolones, tetracyclines, penicillins, macrolides, nitroimidazoles, cephalosporins, diaminopyrimidines, and amphenicol, in animal-derived food products. The method used modified QuEChERS and liquid chromatography coupled to quadrupole-Orbitrap high-resolution mass spectrometry (LC-Q-Orbitrap HRMS). The method was validated in accordance with Commission Implementing Regulation (CIR) EU 2021/808 at five different concentrations ranging from 0.075 to 10,000μgkg-1. The mean recoveries ranged from 58 to 123%, while repeatability values were all below 21%. The calibration curves showed good linearity, with correlation coefficients (R2) ranging from 0.9905 to 0.9999. The limits of detection (LOD) and limits of quantification (LOQ) were in the range of 0.005-43.0μgkg-1 and 0.008-71.7μgkg-1, respectively. The decision limit (CCα) and detection capability (CCβ) ranges were 0.37-2,347µg/kg and 0.44-3,099µg/kg, respectively. Out of the 1,330 samples collected from Egyptian local markets, 1.20% had antibiotic residues. The applicability of the developed method was proven through successful four proficiency testing (PT). The proposed method was demonstrated to be reliable for the simultaneous analysis of multiclass veterinary drugs in bovine liver, muscle tissue, and milk.