A simple and low-cost method using solid-phase extraction and liquid chromatography with UV detection was developed to quantify six alkaloids—N,N-dimethyltryptamine, tryptamine, harmine, harmaline, harmalol, and tetrahydroharmine—in ayahuasca samples. The method demonstrated good linearity and repeatability, with a detection limit of 0.12 mg/L. It was applied to 20 samples from a religious group in Fortaleza, Brazil, revealing alkaloid concentrations ranging from 0.3 to 36.7 g/L.
A solid-phase extraction method using ultra-performance liquid chromatography-tandem mass spectrometry was developed to quantify five major alkaloids—N,N-dimethyltryptamine, harmine, harmaline, harmalol, and tetrahydroharmine—in ayahuasca. Two new adsorbent materials, coconut charcoal and menthone-thiosemicarbazone polymer, were tested. Recoveries ranged from 40.6% to 116.2%, with detection limits between 0.003 and 0.016 μg mL⁻¹ and quantification limits between 0.009 and 0.043 μg mL⁻¹. The method was linear over 0.05–1.0 μg mL⁻¹ (correlation coefficients 0.9969–0.9998). Applied to an ayahuasca sample from a religious group in Fortaleza, Brazil, alkaloid concentrations ranged from 0.3 to 19.3 mg mL⁻¹.