SIMULTANEOUS DETERMINATION OF LINCOMYCIN AND FIVE MACROLIDE ANTIBIOTIC RESIDUES IN HONEY BY LIQUID CHROMATOGRAPHY COUPLED TO ELECTROSPRAY IONISATION MASS SPECTROMETRY

International audienceA sensitive and specific method based on liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), for the simultaneous determination of lincomycin and five macrolide antibiotics in honey, was developed and validated. The analytes were extracted with Tris buffer 0.1 M pH 10.5 and cleaned-up by a single solid phase extraction step on OASIS HLB column. The chromatographic separation of analytes was performed on a Synergi Hydro-RP reversed – phase column using a gradient program of aqueous 0.01 M ammonium acetate pH 3.5 and acetonitrile as the mobile phase, at a flow rate 0.25 ml min –1. Detection of analytes was achieved by positive ionisation electrospray in Multiple Reaction Monitoring (MRM) mode. Two characteristic transitions were monitored for each substance. The following analytical parameters were validated according to the guidelines laid down by Commission Decision 2002/657/EC: linearity, specificity, decision limit (Cca), detection capability (Ccb), repeatability, within-laboratory reproducibility, recovery and ruggedness