A rapid, simple, and strongly selective miniaturized solid phase extraction (SPE) technique, requiring only small amounts of sorbent (24 mg) and elution solvent (600 μL), coupled with ultrahigh-performance liquid chromatography and quadrupole time-of-flight mass spectrometry was developed for detecting tetracycline antibiotics. These analytes were extracted from honey and milk using chitosan-modified graphitized multiwalled carbon nanotubes (G-MWNTs) as the solid sorbent and acetonitrile/acetic acid (8:2, v/v) as the eluent in miniaturized SPE. Under the optimum experimental conditions, a satisfactory linearity (r(2) > 0.992) was obtained, and the limits of detection were in the range of 0.61-10.34 μg/kg for the analytes. The mean recoveries of the five tetracycline antibiotic residues in the real samples were between 81.5 and 101.4%. The results demonstrated that chitosan-modified G-MWNTs comprise a promising material for the enrichment of tetracycline antibiotics from complex food matrices.
Keywords: chitosan; graphitized multiwalled carbon nanotubes; miniaturized solid phase extraction; quadrupole time-of-flight mass spectrometry; tetracycline antibiotics; ultrahigh-performance liquid chromatography.