Assessment of tropane alkaloid levels in Brazilian buckwheat flour products: A novel LC-UHPLC-MS/MS approach using solid-liquid extraction at low temperature.

• Tropane alkaloids (TAs) can contaminate crops and food. • Buckwheat is vulnerable to tropane alkaloid contamination. • Hyoscyamine and scopolamine were determined in food using bidimensional chromatography. • TAs were extracted using solid-liquid extraction at low temperature. • TAs were not detected in Brazilian buckwheat flour (18 samples analyzed) In recent years, the monitoring of tropane alkaloids, specifically hyoscyamine and scopolamine, in food has become a pressing concern. This is due to increasing reports of food contamination with these compounds worldwide, raising awareness about the potential risks associated with their consumption. A novel method is proposed here for the determination of the sum of (+)-hyoscyamine, (–)-hyoscyamine, and (–)-scopolamine in buckwheat-based matrices, using solid-liquid extraction at low temperature and quantification by bidimensional chromatography coupled to tandem mass spectrometry. The validated method presented a linear response in the concentration range of 2.5–15 μg kg−1 (r > 0.99). The precision and accuracy were in the ranges from 0.8 to 11.0 % and from 96 to 103 %, respectively. The limit of quantification (LOQ) was 2.5 μg kg−1. No contamination was found at levels above the LOQ in any of the 18 samples analyzed (buckwheat flour, grains, and gluten-free mix). [ABSTRACT FROM AUTHOR]