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

Currently, the analysis of trace-level contaminants in food must be addressed following green analytical chemistry principles and with a commitment to the sustainable development goals. Accordingly, a sustainable and ecofriendly microextraction procedure based on μ-SPEed followed by ultrahigh 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 -oxide, lasiocarpine, echimidine, and echimidine -oxide were the main pyrrolizidine alkaloids in the samples analyzed.