An Efficient Ambient Ionization Mass Spectrometric Approach to Detection and Quantification of the Mescaline Content of Commonly Abused Cacti from the Echinopsis Genus

Abstract

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Detection and Quantification of Psychoactive N,N-Dimethyltryptamine in Ayahuasca Brews by Ambient Ionization High-Resolution Mass Spectrometry

“…The US Food and Drug Administration (FDA) Guidelines for the Development and Validation of Bioanalytical Methods have been used to validate DART-HRMS protocols to quantify the psychoactive molecules in commercial botanical products and plant preparations. − These guidelines include: (1) demonstration that the method is selective, sensitive, and reproducible; (2) development of standard curves using a minimum of six nonzero calibrators; (3) a blank calibrator and a zero calibrator (i.e., a blank calibrator with internal standard) that do not interfere with the analyte of interest and do not exceed 5% of the average responses in the curve calibrators and quality control (QC) standards; (4) the lowest point of the standard curve being the lower limit of quantification (LLOQ); and (5) utilization of QC standards at four levels (high, medium, low, and LLOQ) incorporated into the curve . Criteria that an analysis must meet to be declared validated are as follows: (1) nonzero calibrators should be within 15% of nominal (theoretical) concentrations, except for the LLOQ calibrator, which can be within 20% of its nominal value; (2) 75%, and a minimum of six nonzero calibrators are required to meet the previous guideline; (3) ≥67% of the QC standards should be within 15% of their nominal values; and (4) ≥50% of the QC standards at each level must be within 15% of their nominal values .…”

“…The dramatic rise in law enforcement encounters with ayahuasca and the plants from which it is made, particularly in a forensic context, have increased the demand for methods to assist forensic crime labs in the efficient analysis and identification of the plant ingredients, as well as the ayahuasca beverage itself. Although reports of quantification of psychoactive molecules for forensic purposes have become more prevalent with the increasing recreational use of the plants identified by the UNODC, − few reports involve the quantification of these molecules in plant-based complex mixtures. Various gas chromatography- (GC) ,,− and liquid chromatography-mass spectrometry (LC-MS) ,,,− methods have been developed for the analysis of ayahuasca and quantification of DMT in the plant material and brews.…”

Quantification of hordenine in a complex plant matrix by direct analysis in real time–high‐resolution mass spectrometry: Application to the “plant of concern” Sceletium tortuosum

“…DART-HRMS has successfully been used to quantify psychoactive materials in other plants of concern including N,N-dimethyltryptamine in ayahuasca brews, 19 yangonin in kava, 20 mitragynine in kratom, 21 and mescaline in various cacti, 22…”

“…With the extensive sample preparation and long run times per sample associated with previously used techniques, the ability to quantify the amount of hordenine present, specifically in various complex forms of S. tortuosum , using a rapid technique such as DART‐HRMS would be extremely beneficial. DART‐HRMS has successfully been used to quantify psychoactive materials in other plants of concern including N , N ‐dimethyltryptamine in ayahuasca brews, 19 yangonin in kava, 20 mitragynine in kratom, 21 and mescaline in various cacti, 22 thereby adding to the growing list of validated protocols that crime labs can use to quantify psychoactive compounds by DART‐HRMS. Herein, we describe the development of a validated protocol for the quantification of hordenine via DART‐HRMS and demonstrate its efficient application to the determination of hordenine levels in several commercially available S. tortuosum products.…”

Rapid, novel screening of toxicants in poison baits, and autopsy specimens by ambient mass spectrometry

“…DART-HRMS is characterized by the direct introduction of samples at ambient conditions into the mass spectrometer without prior chromatographic separation ( Gross, 2014 ). Among multiple applications, it was successfully employed in forensic toxicology ( Musah et al, 2012 ; Duvivier et al, 2014 ; Chen et al, 2016 ; Coon et al, 2019 ; Longo and Musah et al, 2020 ; Pozzato et al, 2020 ; Chambers and Musah, 2022 ), food spoilage ( Massaro et al, 2021a ; Massaro et al, 2021b ; Tata et al, 2022a ), and drug analysis ( Schurek et al, 2008 ). In the present study, we captured the presence of 40 different toxicants and one bitter compound (denatonium benzoate) in autopsy specimens and baits.…”