Development and validation of a multiclass method for the analysis of antibiotic residues in eggs by liquid chromatography-tandem mass spectrometry

A multiclass method for the analysis of residues, in egg matrices, of 41 antimicrobial agents belonging to seven families (sulfonamides, diaminopyridine derivates, quinolones, tetracyclines, macrolides, penicillins and lincosamides) was developed and validated according to the requirements of European Commission Decision 2002/657. Compounds were extracted with a pressurized liquid extraction (PLE) technique using a 1:1 mixture of acetonitrile and a succinic acid buffer (pH 6.0) at 70 °C. As this resulted in clear extracts, no further clean-up was necessary. Analytes were determined by ultra-high-pressure liquid chromatography–tandem mass spectrometry (UHPL–MS/MS) in a chromatographic run of 13 min. Calibration was carried out with spiked blank samples subjected to the entire analytical procedure. Five compounds, two of them isotopically labelled, were used as internal standards. Most analytes were quantified with errors below 10%. Precision in terms of reproducibility standard deviation was between 10% and 20% in most cases. CCα values were in the range 0.5–3.8 μg kg⁻¹ for the non-authorized compounds. The proposed method would enable an experienced analyst to process about 25 samples per day.