Multiresidue method for the simultaneous determination of veterinary medicinal products, feed additives and illegal...

A multiclass method was developed for the simultaneous determination of 120 analytes in fresh eggs. The method covers the analytes from the groups of tetracyclines (6), fluoroquinolones (11), sulphonamides (17), nitroimidazoles (9), amphenicols (2), cephalosporins (7), penicillins (8), macrolides (8), benzimidazoles (20), coccidiostats (14), insecticides (3), dyes (12) and others (3). Samples were extracted using 0.1% formic acid in acetonitrile:water (8:2) with the addition of EDTA and cleaned using solid phase extraction with Hybrid SPE cartridges. The chromatographic separation was achieved on C8 column using mobile phase consisting of (A) methanol:acetonitrile (8:2) - (B) 0.1% formic acid in a gradient mode. Validation results according to the Commission Decision 2002/657/EC are as follows: linearity (r⩾0.99), recovery (75-108%), repeatability (CV 1.60-15.9%), reproducibility (CV 2.60-15%), decision limit (CCα 2.25-1156 μg/kg) and detection capability (CCβ 2.04-1316 μg/kg). The presented method was used for analysis of 150 real eggs samples taken from monitoring control program.