Novel online-SPE configured UHPLC-MS/MS analysis to demystify the pyrrolizidine alkaloid contents of honey and bee pollen samples


Akyıldız İ. E., Uzunöner D., Daştan T., Raday S., Acar S., KÖK YETİMOĞLU E., ...Daha Fazla

Food Chemistry, cilt.493, 2025 (SCI-Expanded) identifier identifier

  • Yayın Türü: Makale / Tam Makale
  • Cilt numarası: 493
  • Basım Tarihi: 2025
  • Doi Numarası: 10.1016/j.foodchem.2025.145879
  • Dergi Adı: Food Chemistry
  • Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus, Academic Search Premier, PASCAL, Aerospace Database, Aquatic Science & Fisheries Abstracts (ASFA), BIOSIS, CAB Abstracts, Chemical Abstracts Core, Chimica, Communication Abstracts, Compendex, EMBASE, Food Science & Technology Abstracts, Metadex, Veterinary Science Database, Civil Engineering Abstracts
  • Anahtar Kelimeler: Bee pollen, Honey, LC-MS, Online-SPE, Pyrrolizidine alkaloids
  • Marmara Üniversitesi Adresli: Evet

Özet

Pyrrolizidine alkaloids (PAs) and their N-oxides (PANOs) which might be incorporated into the bee products may pose health risks for consumers. We aimed to analyze PAs of honeys and bee pollens by quantifying 28 PAs/PANOs using a novel online SPE-UHPLC-MS/MS methodology. Dilute & shoot preparation was optimized for honeys, whereas pollen PAs were extracted using ACN/McIlvaine-EDTA buffer. C18-E cartridge was employed for online analyte enrichment and clean-up. Validation results were consistent with the guideline requirements. Samples were botanically categorized and analyzed to clarify PAs' sources. Total concentrations of PAs/PANOs in honey ranged between 0.28 and 177.38 μg/kg; for bee pollens, it was found between 10.9 μg/kg to 14.543 mg/kg. The sum of PAs was higher than 500 μg/kg in 21.2 % of the pollens, which meant these samples exceeded EU criteria. Automated online-SPE strategy allowed us to integrate fast and effortless pretreatment combined with accurate and sensitive PA monitoring.