Simultaneous determination of lincomycin and five macrolide antibiotic residues in honey by liquid chromatography coupled to electrospray ionization mass spectrometry (LC-MS/MS).
A sensitive and specific method based on high-performance 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 programme 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. The detection of analytes was achieved by positive ionization electrospray in multiple reaction-monitoring mode. Two characteristic transitions were monitored for each substance. The following analytical parameters were validated according to the guidelines laid down by European Commission Decision 2002/657/EC (European Commission 2002): linearity, specificity, decision limit (CCalpha), detection capability (CCbeta), repeatability, within-laboratory reproducibility, recovery and ruggedness.
Benetti
C
C
Istituto Zooprofilattico Sperimentale delle Venezie, Viale dell'Università, 10, I-35020, Legnaro (PD), Italy. cbenetti@izsvenezie.it
Piro
R
R
Binato
G
G
Angeletti
R
R
Biancotto
G
G
D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis; D006722:Honey / Q000032:analysis*; D008034:Lincomycin / Q000032:analysis*; D018942:Macrolides / Q000032:analysis; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
D000900:Anti-Bacterial Agents; D018942:Macrolides; D008034:Lincomycin