A dispersive liquid-liquid microextraction method for the determination of ayahuasca alkaloids (N,N-dimethyltryptamine and β-carbolines) in human hair.
Fabiana Pereira Santos, Beatriz Aparecida Passos Bismara Paranhos, Thaisa Meira Sandini, Vítor Bruno, Mauricio Yonamine
Talanta January 27, 2026 DOI: 10.1016/j.talanta.2026.129455 (opens in new tab)
Study at a glance
AI-extracted from the abstract| Characteristics | Method development and validation study Peer reviewed |
|---|---|
| Sample size | 6 |
| Population | Human hair samples from individuals who had consumed ayahuasca |
| Topics | Ayahuasca DMT 5-MeO-DMT |
| Keywords | Dispersive liquid-liquid microextraction Green analytical toxicology Β-carbolines |
| Key points | The developed DLLME-LC-MS/MS method successfully quantified DMT and β-carbolines in human hair, with β-carbolines generally detected at higher concentrations than DMT. |
Abstract
Ayahuasca, a traditional Amazonian hallucinogenic plant brew once used in healing rituals, is now globally popular, raising safety concerns outside ceremonial contexts. Its compounds, alkaloids, are stimulating scientific interest for their potential antidepressant and anxiolytic effects. In this study, we employed a more sustainable analytical extraction method for the determination of N,N-dimethyltryptamine (DMT), harmine (HRN), harmaline (HRL), and tetrahydroharmine (THH) in human hair using LC-MS/MS. We incorporating dispersive liquid-liquid microextraction (DLLME) in line with the principles of Green Analytical Toxicology (GAT). The limit of quantification (LoQ) was 3 pg/mg for HRN and 8 pg/mg for DMT, HRL, and THH. The method was linear in the LoQ range up to 1000 pg/mg (r2 ≥ 0.99). Intra- and inter-day precision and accuracy met the acceptance criteria at three quality control (QC) levels. Matrix effect (EM) showed both ionization enhancement and suppression, values ranged from 80.20 % (DMT, CQB) to 121.85 % (HRL, CQA). Recovery (RE) was low with recovery values ranging from 36.28 % to 57.91 %. Selectivity studies revealed no interference. Application to six authentic samples confirmed the viability of the method. Measured concentrations were DMT (21.5-204.4 pg/mg) and β-carbolines: THH (55.5 - >LOQ pg/mg); HRL (42.0-988.2 pg/mg) and HRN (163.0 - >LOQ pg/mg). Notably, β-carbolines were generally detected at higher concentrations than DMT. The proposed method uses smaller amounts of organic solvents compared to conventional hair extraction methods, representing a significant methodological advancement in the analysis of psychoactive alkaloids in biological matrices.