UHPLC-Q-TOF analysis of pyrrolizidine alkaloids in North-Macedonian honey

ABSTRACT

Honey contaminated with pyrrolizidine alkaloids (PAs) could pose a risk for human consumption, being a widely consumed food product. A fast and simple LC/MS method for the analysis of pyrrolizidine alkaloids in honey was optimised to collect occurrence data. The extraction efficiency was evaluated by a systematic study of multiple solvent mixtures and clean-up procedures. The best results for PA extraction were obtained using a formic acid/methanol mixture with subsequent clean-up by the QuEChERS method, resulting in a mean recovery range of 91.8–102%. The method validation showed satisfactory intra-day (RSD < 5.1%) and inter-day precision (RSD < 9.1%). The proposed method was applied to 14 samples. A total of six PAs and two N-oxides were detected, with levels between 89 and 8188 µg/kg. This assessment highlights the potential risk of intoxication and the need for further investigations regarding an effective quality system for manufacturers to control PAs in honey.

KEYWORDS:

• Pyrrolizidine alkaloids (PAs)
• UHPLC-Q-TOF
• honey
• food safety
• extraction efficiency
• clean-up

Acknowledgments

The authors gratefully acknowledge the financial support provided by the OPCW for the project titled: “Risk Analysis of Natural Toxic Pyrrolizidine Alkaloids in the Food Chain: Development, Validation and Application of HPLC/MSⁿ Methods”, Grant L/ICA/ICB/222477/20. The authors also express gratitude to CEEPUS M-RO-0010-2223-165681 “Teaching and Learning Bioanalysis” Network for the mobility grants that made possible the North Macedonian-Croatian cooperation in this paper.

Disclosure statement

No potential conflict of interest was reported by the author(s).

Supplementary material

Supplemental data for this article can be accessed online at https://doi.org/10.1080/19393210.2023.2266701.

Additional information

Funding

This work was supported by the “Teaching and Learning Bioanalysis” Network for the mobility grants [CEEPUS M-RO-0010-2223-165681]; Risk Analysis of Natural Toxic Pyrrolizidine Alkaloids in the Food Chain: Development, Validation, and Application of HPLC/MSn Methods, supported by the OPCW [L/ICA/ICB/222477/20].