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

Food Addit Contam Part B Surveill. 2024 Mar;17(1):5-15. doi: 10.1080/19393210.2023.2266701. Epub 2024 Feb 12.

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; clean-up; extraction efficiency; food safety; honey.

MeSH terms

  • Chromatography, High Pressure Liquid
  • Food Contamination / analysis
  • Honey* / analysis
  • Pyrrolizidine Alkaloids* / analysis
  • Republic of North Macedonia
  • Tandem Mass Spectrometry / methods

Substances

  • Pyrrolizidine Alkaloids