Evaluation of a multiresidue capillary electrophoresis-quadrupole-time-of-flight mass spectrometry method for the determination of antibiotics in milk samples

•Evaluation of CZE-Q-TOF-MS for the determination of 15 antibiotic residues in milks.•Oasis PRiME HLB SPE for the analysis of eight tetracyclines and seven quinolones.•Limits of quantification ranged from 1.5 to 9.6 μg kg−1 and RSD below 13%.•Recoveries in goat, whole and semi-skimmed cow milks from 76 to 106%.

A selective and rapid method has been developed to determine 15 antibiotic residues (eight tetracyclines and seven quinolones) in milk samples by capillary zone electrophoresis coupled with quadrupole time-of-flight mass spectrometry (CZE-Q-TOF-MS). The use of this hybrid mass spectrometer allowed obtaining full scan and full MS/MS spectra for quantification/confirmation purposes in a single run. In addition, solid phase extraction (SPE) using the new Oasis PRiME HLB cartridge was proposed for the extraction, achieving excellent results in terms of sample throughput. The proposed method was validated using whole cow milk as representative matrix. Good linearity was obtained (R2 > 0.99) for all the studied compounds. The precision, expressed as relative standard deviation (%, RSD), at two concentration levels (50 and 100 μg kg−1) was below 13%. Recoveries obtained from goat milk, whole cow milk and semi-skimmed cow milk, at two concentration levels, ranged from 76 to 106%, while limits of quantification ranged from 1.5 to 9.6 μg kg−1, being lower than the established maximum residue limits in the European legislation. Matrix effect was negligible in all cases, showing that with this new SPE sorbent cleanest extracts were obtained with a minimum number of steps in the sample treatment. Thus, the proposed SPE-CZE-Q-TOF-MS method is suitable for multiclass multiresidue monitoring in different types of milk samples.