A Rapid Ultrasound–Vortex-Assisted DLLME–GC–IT/MS Method for Multiclass Determination of Organic Contaminants in Honey

Honey is recognized as a valuable tool for environmental biomonitoring, while its contaminant content is relevant to food safety, requiring analytical methods for the simultaneous determination of multiple contaminants. In this study, an ultrasound–vortex-assisted dispersive liquid–liquid microextraction (UVA-DLLME) procedure coupled with gas chromatography–ion trap mass spectrometry (GC–IT/MS) was developed for the simultaneous determination of pesticides, polycyclic aromatic hydrocarbons (PAHs), and polychlorinated biphenyls (PCBs) in honey. The extraction solvent composition was optimized using different n-heptane/toluene mixtures, and the selected conditions were validated in terms of linearity, recovery, sensitivity, and precision. The optimized method provided recoveries between 70.2 and 112%, coefficients of determination (R2) from 0.9389 to 0.9998, limits of detection ranging from 0.40 to 21 ng g−1, and intraday and interday relative standard deviations below 15%. The environmental performance of the sample preparation procedure was evaluated using the AGREEprep metric, giving an overall score of 0.52. Application of the method to 21 artisanal honey samples showed a generally low occurrence of the investigated contaminants, with PAHs being the most frequently detected compounds, whereas pesticides and PCBs were mostly below the limits of detection or quantification. The proposed method represents a solvent-efficient analytical procedure suitable for the multiclass determination of organic contaminants in honey.