Development and validation of a new method for the simultaneous determination of spinetoram J and L in honey from different botanical origins employing solid-phase extraction with a polymeric sorbent and liquid chromatography coupled to quadrupole time-of-flight mass spectrometry

Abstract

The objective of this study was to propose a novel method to determine residues of the bio-insecticide spinetoram, which is a mixture of two components (spinetoram J and L), in honey from multifloral, rosemary and heather botanical origins; liquid chromatography coupled to quadrupole time-of-flight mass spectrometry was the technique employed. An efficient sample treatment (recoveries between 82% and 95%) involving a solid-phase extraction with a polymeric sorbent has been recommended, and no matrix effect was observed. Chromatographic analysis (4 min) was performed in reverse phase mode by using a fused-core column (Kinetex® EVO C₁₈) with acetonitrile and ammonium formate as the mobile phase components, which was applied in isocratic elution mode. Method was validated according to the current European legislation. Not only was it selective, but it also displayed a wide linear range, good precision (relative standard deviation values lower than 9%) and sensitivity (low limits of detection (spinetoram J, 0.1-0.3 μg/kg; spinetoram L, 0.1-0.2 μg/kg) and quantification (spinetoram J, 0.3-1.2 μg/kg; spinetoram L, 0.4-0.7 μg/kg)). Several honey samples were analyzed with this method and no spinetoram residues were found above the limits of detection.

Keywords: Food analysis; Honey; Insecticides; LC-Q-TOF/MS; Method validation; Polymeric sorbents; Solid-phase extraction; Spinetoram.