Use of Coconut Charcoal and Menthone-Thiosemicarbazone Polymer as Solid Phase Materials for the Determination of N,N-Dimethyltryptamine, Harmine, Harmaline, Harmalol, and Tetrahydroharmine in Ayahuasca Beverage by Liquid Chromatography-Tandem Mass Spectrometry

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.

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Abstract

An extraction method based on solid-phase extraction was developed to determine the major alkaloid components, N,N-dimethyltryptamine, harmine, harmaline, harmalol, and tetrahydroharmine, in ayahuasca using ultra-performance liquid chromatography-tandem mass spectrometry.Coconut charcoal and menthone-thiosemicarbazone polymer were tested as new adsorbent materials.Experiments carried out at levels of 1, 5, 10, 50, 100, and 250 μg mL -1 resulted in recoveries in the ranges 45.3-115.7%for menthone-thiosemicarbazone and 40.6-116.2%for coconut charcoal.The detection and quantification limits ranged from 0.003 to 0.016 μg mL -1 and from 0.009 to 0.043 μg mL -1 , respectively.The method developed was linear over the tested range (0.05-1.0 μg mL -1 ), with correlation coefficients ranging from 0.9969 to 0.9998.The technique was applied for analysis of the compounds in an ayahuasca sample collected from a religious group located in the city of Fortaleza, obtaining concentrations in the range from 0.3 to 19.3 mg mL -1 .