Comparative contaminant and chemical profiling of commercial yerba mate infusions prepared as chimarrão and tereré from Southern Common Market countries.

Yerba mate (Ilex paraguariensis A. St.-Hil.) is widely consumed in South America and contains diverse naturally occurring compounds, while potentially hazardous contaminants may be introduced during cultivation, processing, and commercialization. In this study, a direct immersion solid-phase microextraction coupled with single-quadrupole gas chromatography-mass spectrometry (DI-SPME/GC-MS) method was developed for targeted determination of selected phthalates and pesticides and untargeted chemical profiling of commercial yerba mate from Southern Common Market (MERCOSUL) countries (Paraguay, Argentina, Brazil, and Uruguay). Extraction conditions were evaluated using a factorial design, identifying agitation speed and salt addition as the most influential variables. The method showed satisfactory analytical performance, with R² > 0.99, recoveries of 84-104%, relative standard deviations (RSDs) below 8%, and limits of detection of 0.31-3.04 μg L⁻¹. Analysis of 48 commercial samples revealed frequent occurrence of phthalates and pesticides, with dibutyl phthalate (DBP) showing the highest detection frequency (67%). Untargeted GC-MS screening identified 476 and 673 compounds in tereré and chimarrão, respectively, with greater chemical diversity in the hot infusion. Principal component analysis (PCA) and hierarchical cluster analysis (HCA) identified preparation temperature as the main factor associated with sample discrimination, while country of origin and drying conditions showed secondary effects. Naturally occurring compounds, polycyclic aromatic hydrocarbons (PAHs), and phthalate-related compounds were detected, suggesting contributions from smoke-drying and packaging-related contamination. These findings demonstrate the suitability of DI-SPME/GC-MS for contaminant monitoring and chemical profiling of yerba mate infusions.