The stem bark of Tetrapterys mucronata, a plant used in Brazilian ayahuasca preparations, contains four tryptamine alkaloids with known toxic and hallucinogenic properties. Quantitation by HPLC-ESI/MS/MS in ethanolic extracts found bufotenine at 3.26 mg/g, 5-methoxy-N-methyltryptamine at 0.88 mg/g, 5-methoxy-bufotenine at 3.07 mg/g, and 2-methyl-6-methoxy-1,2,3,4-tetrahydro-β-carboline at 0.14 mg/g. A water decoction mimicking ayahuasca showed slightly lower levels, with bufotenine at 2.32 mg/g and 5-methoxy-bufotenine at 1.53 mg/g. These significant alkaloid levels, particularly of bufotenine and 5-methoxy-bufotenine, indicate that consuming this plant in ayahuasca may pose a risk to consumers.
Three miniaturized extraction techniques—dispersive liquid-liquid microextraction (DLLME), microextraction by packed sorbent (MEPS), and QuEChERS—were compared for extracting the main ayahuasca compounds (DMT, tetrahydroharmine, harmine, harmaline, harmol, and harmalol) from beverage samples. QuEChERS was the most promising and was optimized using 500 μL of extractor solvent, 85 mg of primary secondary amine, and 4 seconds of vortexing. The validated method showed linear ranges of 0.16–10 μg/mL for β-carbolines and 0.016–1 μg/mL for DMT, with extraction efficiencies between 60.2% and 88.0%. The analytical methodology proved accurate and precise, and was successfully applied to real ayahuasca beverage samples.