Abstract
Ayahuasca tea is an entheogen hallucinogenic beverage used for shamanic and spiritual purposes, prepared by the decoction of different Amazonian plants containing N,N-dimethyltryptamine (DMT) and harmala alkaloids. Since the therapeutic potential of this tea has been broadly studied in recent years, mainly for the treatment of psychiatric disorders, the determination of the ayahuasca tea components in human and animal matrices is of utmost importance. In order to avoid the use of large amounts of toxic solvents, typically employed in traditional sample preparation methods, hollow fiber liquid-phase microextraction (HF-LPME) presents a greener and time-saving alternative. The present study aims to fully develop and apply an HF-LPME method for the determination of DMT, harmine (HRM), harmaline (HRL), and tetrahydroharmine (THH) in human urine samples using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Fractional factorial and Box–Behnken designs were used to identify and optimize significant method variables. Once optimized, validation has shown a limit of detection (LoD) of 1.0 ng/ml for DMT and 2.0 ng/ml for the harmala alkaloid. The limit of quantification (LoQ) was of 5.0 ng/ml for all analytes. The method has shown to be linear over a concentration range of 5–200 ng/ml (r2 ≥ 0.99). Intra/inter-day precision and accuracy met the acceptance criteria at the three quality control (QC) levels studied (15.0, 90.0, and 170.0 ng/ml, n = 6, each). Matrix effect evaluation showed predominant ion enhancement and recovery values were above 80%. Dilution factors of 10- and 20-fold have shown acceptable values of accuracy. Selectivity studies showed no interferences. Analysis of eight authentic samples collected from four subjects proved method feasibility. A simple, time-saving and green alternative for the analysis of DMT and harmala alkaloids in human urine samples was developed, optimized using design of experiments, fully validated and applied to authentic samples.
Highlights
Ayahuasca tea is an entheogen preparation historically used by the indigenous people from the Amazon Basin region for at least 1,000 years (Callaway et al, 1999; Miller et al, 2019; Orsolini et al, 2020)
The use of hollow fiber liquid-phase microextraction (HF-LPME) has been shown to offer a great performance and considering the importance of quantifying ayahuasca alkaloids in biological matrices, this study presents a fast HF-LPME method followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLCMS/MS) for the determination of DMT, THH, HRL, and HRM in human urine samples
Chromatographic separation is not mandatory when using monitoring mode (MRM), special attention was given to HRL and HRM separation since initial experimentation has demonstrated possible ion suppression for HRL when overlapped with HRM
Summary
Ayahuasca tea is an entheogen preparation historically used by the indigenous people from the Amazon Basin region for at least 1,000 years (Callaway et al, 1999; Miller et al, 2019; Orsolini et al, 2020). The improvement in the sensitivity of chromatographic and mass spectrometry techniques has resulted in the need for less laborious sample preparation methods, such as diluteand-shoot (Bjornstad et al, 2009; Mcilhenny et al, 2011; Pope et al, 2019) and protein precipitation (Zhao et al, 2012; Meyer et al, 2014; de Morais et al, 2018) approaches, which use very small amounts of urine These simple, faster, cheaper, and less hazardous methodologies have become prominent in the analysis of ayahuasca alkaloids. 36 22 11 29 17 29 17 13 41 33 25 41 33 25 analysis of eight authentic samples donated by four individuals after a usual ayahuasca ceremony
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