Comprehensive profiling and risk assessment of glycoalkaloids and their aglycones in commercial potato-based snacks using miniaturized extraction and purification coupled with UHPLC-MS/MS

Abstract

Glycoalkaloids (GAs) are naturally occurring compounds in Solanum species whose occurrence, transformation, and cumulative exposure in processed foods remain poorly characterized. This study provides a risk assessment framework based on ultrasound-assisted extraction and vacuum manifold-assisted pipette tip solid-phase extraction coupled with UHPLC-MS/MS. By enabling the simultaneous determination of major and minor potato- and tomato-derived GAs, and their aglycones in a single workflow, the method represents a significant advancement over conventional approaches. The method demonstrated high analytical performance (recoveries 87–105%) and sustained efficiency of the mesostructured MSU-2-C18 sorbent over 15 reuse cycles, highlighting high-throughput routine monitoring. Application to 30 commercially available potato-based snacks revealed pronounced variability in total GAs (0.8 ± 0.3 – 42 ± 2 mg/kg), with higher levels in potato chips than in extruded snacks. In addition, this study shows the presence of γ-chaconine (up to 17.5%) and the aglycone solanidine (up to 22.8%), in highly processed matrices. In extruded potato snacks with tomato-derived ingredients, α tomatine and tomatidine were selectively detected, with tomatidine accounting for 25–80% of the combined amount of both compounds, demonstrating the coexistence of other sources of exposure to GAs. The Margin of Exposure (MOE) was evaluated under different exposure scenarios for adults and children. Overall, MOE values indicated no health concern across all evaluated scenarios, remaining above the safety threshold. The only exception was one potato chip sample, which yielded an MOE of 9 for children (14.3 kg body weight) under the high scenario (consumption of 40g), suggesting a potential health concern