Abstract:

A method using mixed-mode ion exchange liquid chromatography-tandem mass spectrometry was developed for the determination of streptomycin, dihydrostreptomycin, spectinomycin, kanamycin and amikacin in honey. The honey samples were extracted with phosphate followed by clean-up with SupelMIP Aminoglycosides SPE cartridges. The separation was performed on an SIELC Obelisc R column (100 mm×2.1 mm, 5 μm) by the gradient elution program using 0.1%(v/v) formic acid aqueous solution and acetonitrile as the mobile phases, at a flow rate of 0.4 mL/min. Five aminoglycosides (AGs) were identified by the tandem mass spectrometer with an electrospray ionization source under the multiple reaction monitoring (MRM) mode. The quantification analysis was performed by the external standard method. The calibration curves showed good linearity in the range of 5-100 μg/L for streptomycin and dihydrostreptomycin, and 20-500 μg/L for spectinomycin, kanamycin and amikacin. The limits of quantification (LOQs) of the five drugs in honey were 5-20 μg/kg. The average recoveries of the five drugs from feeds spiked at LOQ, 2-fold LOQ and 5-fold LOQ levels were 75.1%-92.3%, and the relative standard deviations (RSDs) were 4.5%-10.7%. The method is simple, rapid, and sensitive, and is suitable for the simultaneous determination of the five aminoglycoside residues in honey.

Key words: aminoglycoside, honey, mixed-mode ion exchange liquid chromatography-tandem mass spectrometry