Simultaneous determination of lincomycin and five macrolide antibiotic residues in honey by liquid chromatography coupled to electrospray ionization mass spectrometry (LC-MS/MS)

Abstract

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 (CCα), detection capability (CCβ), repeatability, within-laboratory reproducibility, recovery and ruggedness.

Keywords:

• Lincomycin
• macrolides
• honey
• validation
• high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)