Multiclass screening method based on solvent extraction and liquid chromatography–tandem mass spectrometry for the determination of antimicrobials and mycotoxins in egg

A QuEChERS (Quick Easy Cheap Effective Rugged Safe)-like extraction method was developed for the simultaneous analysis of veterinary drugs and mycotoxins in hen eggs by liquid chromatography–tandem mass spectrometry (LC–MS/MS) with electrospray (ESI) source. Various classes of antimicrobials (tetracyclines, ionophores, coccidiostats, penicillins, cephalosporins, fluoroquinolones, sulfonamides) and mycotoxins (enniatins, beauvericin, ochratoxins, aflatoxins) were considered for the development of this method. Particular attention was devoted to extraction optimization: different solvents (acetone, acetonitrile and methanol), different pH values and different sample to extracting volume ratios were tested and evaluated in terms of recovery, relative standard deviation (RSD) and ESI signal suppression due to matrix effect. Chromatographic and mass spectrometric conditions were optimized to obtain the best instrumental performances for most of the analytes. Quantitative analysis was performed by means of matrix-matched calibration, in a range that varied depending on the analyte and its established maximum limit, when there was one. Recoveries at 100 μg kg−1 spiking level were >62% (3 < RSD < 17) for all the antimicrobials except lasalocid A (41 ± 10%) and oxacillin (56 ± 17%). The multiclass method proposed is rapid, simple, and involves a low solvent consumption, in line with QuEChERS features and modern analytical requirements.

► Simultaneous determination of antimicrobials and mycotoxins in egg.
► Evaluation of extraction conditions by factorial experimental design.
► Simple QuEChERS-like extraction with low cost, solvent consumption and analysis time.