Determination of pesticides and persistent organic pollutants in honey by accelerated solvent extraction and GC-MS/MS

Importance of the Topic

Honey is valued for its nutritional and medicinal attributes but is vulnerable to contamination by persistent organic pollutants and pesticides used in apiculture and agriculture.
Monitoring these residues is crucial for consumer safety and compliance with stringent regulations for organic products.

Objectives and Study Overview

This study aimed to develop and validate a multiresidue analytical method combining accelerated solvent extraction with inline cleanup and GC–MS/MS detection for quantification of PCBs, PBDEs, organochlorine and organophosphorus pesticides, and other agrochemicals in honey.
A total of 59 organic honey samples from three Italian regions (Calabria, Trentino Alto Adige, Lombardia) were analyzed to assess regional contamination profiles.

Methodology and Instrumentation

• Sample Preparation: 2 g honey mixed with dispersant and sodium sulfate, extracted using Thermo Scientific Dionex ASE 350 with Florisil inline cleanup (hexane/ethyl acetate 4:1, 80 °C, 1500 psi).
• Concentration: Rocket Evaporator to 200 μL final volume.
• Analysis: Thermo Scientific TRACE 1310 GC with PTV injector and TSQ 8000 Evo triple quadrupole MS/MS, operated in SRM mode; software: Xcalibur and TraceFinder.
• Quantification: Matrix-matched calibration, LOD/LOQ calculation, recoveries and repeatability evaluated at 10 ng/g.

Main Results and Discussion

• Method performance: Excellent linearity (r² ≥ 0.99), recoveries between 75 % and 105 %, LOQs from 0.03 to 3.36 ng/g, and repeatability CV ≤ 14 %.
• PCBs: Detected in all samples at 0.27–0.92 ng/g with no significant regional differences.
• PBDEs: Not detected, likely reflecting organic production environments.
• Organochlorine pesticides: Endrin, DDT and metabolites, heptachlor, and endosulfan sulfate were found at low ng/g levels, under current MRLs.
• Organophosphorus pesticides: Multiple OPs (e.g., diazinon 1.13–1.15 ng/g, mevinphos, coumaphos) were prevalent in Trentino Alto Adige and Calabria; Captan noted in Lombardia.

Benefits and Practical Applications

The single-step ASE protocol with inline cleanup reduces solvent use, extraction time, and sample handling. Combined with GC–MS/MS, it provides high sensitivity and selectivity for routine monitoring of honey and similar matrices.

Future Trends and Potential Applications

Further development may include expanded analyte panels, application to other food matrices, miniaturized extraction formats, and seamless integration with automated workflows and data analysis platforms.

Conclusion

The validated ASE–GC–MS/MS method offers a rapid, reliable, and environmentally friendly approach for comprehensive profiling of pesticide and POP residues in honey, supporting food safety and regulatory compliance efforts.

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