Miniaturized Analytical Strategy Based on μ‑SPEed for Monitoring the Occurrence of Pyrrolizidine and Tropane Alkaloids in Honey

Abstract

Currently, the analysis of trace-level contaminants in food must be addressed following the Green Analytical Chemistry principles and with the commitment to the Sustainable Development Goals. Accordingly, a sustainable and ecofriendly microextraction procedure based on µ-SPEed® followed by ultra-high liquid chromatography coupled to ion-trap tandem mass spectrometry analysis was developed to determine the occurrence of pyrrolizidine and tropane alkaloids in honey samples. The µ-SPEed® procedure took approximately 3 min per sample, using only 100 μL of organic solvent and 300 μL of diluted sample. The method was properly validated (overall recoveries 72-100% and precision RSD values ≤15%) and its greenness was scored at 0.61 out of 1. The method was applied to different honey samples, showing overall contamination levels from 32 to 177 µg/kg of these alkaloids. Atropine was found in all the samples, whereas retrorsine N-oxide, lasiocarpine, echimidine and echimidine N-oxide were the main pyrrolizidine alkaloids in the samples analyzed.