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

• Published in: Food additives & contaminants Part B, Surveillance communications Vol. 17; no. 1; pp. 5 - 15
• Main Authors: Cvetanoska, Marinela, Pocrnić, Marijana, Stefova, Marina, Galić, Nives, Petreska Stanoeva, Jasmina
• Format: Journal Article
• Language: English
• Published: England Taylor & Francis 01.03.2024; Taylor & Francis Ltd
• Subjects: Alkaloids; Chromatography, High Pressure Liquid; clean-up; European People; extraction efficiency; Food Contamination - analysis; food safety; Formic acid; honey; Honey - analysis; Humans; Mixtures; Pyrrolizidine alkaloids (PAs); Pyrrolizidine Alkaloids - analysis; Tandem Mass Spectrometry - methods; UHPLC-Q-TOF; food safety; Pyrrolizidine alkaloids (PAs); extraction efficiency; honey; clean-up; UHPLC-Q-TOF
• ISSN: 1939-3210; 1939-3229
• DOI: 10.1080/19393210.2023.2266701

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.