Monitoring tropane alkaloids in plant-based beverages using μSPEed® strong cation exchange ordered mesoporous silica cartridges

Abstract

This study introduces a novel miniaturized method using μSPEed® and ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) for the extraction and purification of atropine and scopolamine in plant-based beverages. The approach employs a sorbent of SM-type ordered mesoporous silica functionalized with sulfonic acid groups, packaged for the first time in a miniaturized format. Validation followed Regulation (EU) 2023/2783, demonstrating excellent performance: recoveries (91–105%), precision (RSD ≤19%), linearity (R2 ≥ 0.996), low quantification limits (0.06–0.4 μg/L), slight matrix effect, and proper selectivity. Analysis of 26 commercial samples purchased in Spain revealed contamination in 21 samples. Millet-based beverages, a previously unstudied matrix, showed the highest combined levels of atropine and scopolamine (1.2 μg/L), followed by oat-based (1.1 μg/L) and spelt-based beverages (0.83 μg/L). Maximum concentrations reached 0.80 μg/L for atropine and 1.03 μg/L for scopolamine, highlighting the need for legal limits to improve food safety.