title: Ultra-high-pressure liquid chromatography tandem mass spectrometry determination of hallucinogenic drugs in hair of psychedelic plants and mushrooms consumers.
abstract: A procedure based on ultra-high-pressure liquid chromatography tandem mass spectrometry has been developed for the determination of mescaline, N,N-dimethyltryptamine, psilocin, psilocybin, salvinorin A in hair of consumers of psychedelic vegetal material such peyote or trichocereus cacti, psilocybe mushrooms, Salvia divinorum or psychedelic beverage ayahuasca. After hair washing with methyl alcohol and diethyl ether and subsequent addition of mescaline-d9 and 3,4-methylenedioxypropylamphetamine as internal standards, hair samples were treated with 250μl VMA-T M3 reagent for 1h at 100°C. After cooling, 100μl M3 extract were diluted with 400μl water and a volume of 10μl was injected into chromatographic system. Chromatographic separation was achieved at ambient temperature using a reverse-phase column and a linear gradient elution with two solvents: 0.3% formic acid in acetonitrile and 5mM ammonium formate pH 3. The mass spectrometer was operated in positive ion mode, using multiple reaction monitoring via positive electrospray ionization. The method was linear from the limit of quantification (0.03-0.05ng/mg depending on analyte under investigation) to 10ng/mg hair, with an intra- and inter-assay imprecision and inaccuracy always less than 15% and an analytical recovery between 79.6% and 97.4%, depending on the considered analyte. Using the validated method, mescaline was found in concentration range of 0.08-0.13ng/mg in hair of peyote smokers, 3.2ng salvinorin A per mg hair were determined in hair from a S. divinorum smoker, 5.6ng N,N-dimethyltryptamine per mg hair from an ayahuasca user and finally 0.8ng psilocybin per ng hair of a psilocybe consumer.
authors.affiliation: Drug Abuse and Doping Unit, Department of Therapeutic Research and Medicines Evaluation Istituto Superiore di Sanità, Roma 00161, Italy. Electronic address: simona.pichini@iss.it.
authors.forename: Simona
authors.initials: S
authors.lastname: Pichini
authors.affiliation: Drug Abuse and Doping Unit, Department of Therapeutic Research and Medicines Evaluation Istituto Superiore di Sanità, Roma 00161, Italy.
authors.forename: Emilia
authors.initials: E
authors.lastname: Marchei
authors.affiliation: Unitat de Recerca Infància i Entorn (URIE), Paediatric Service, Institut de Recerca Hospital delMar - IMIM, Barcelona, Spain.
authors.forename: Oscar
authors.initials: O
authors.lastname: García-Algar
authors.affiliation: Unitat de Recerca Infància i Entorn (URIE), Paediatric Service, Institut de Recerca Hospital delMar - IMIM, Barcelona, Spain.
authors.forename: Arelis
authors.initials: A
authors.lastname: Gomez
authors.affiliation: Drug Abuse and Doping Unit, Department of Therapeutic Research and Medicines Evaluation Istituto Superiore di Sanità, Roma 00161, Italy.
authors.forename: Rita
authors.initials: R
authors.lastname: Di Giovannandrea
authors.affiliation: Drug Abuse and Doping Unit, Department of Therapeutic Research and Medicines Evaluation Istituto Superiore di Sanità, Roma 00161, Italy.
authors.forename: Roberta
authors.initials: R
authors.lastname: Pacifici
mesh_terms: D000363:Agaricales / Q000737:chemistry*; D002021:Buffers; D002138:Calibration; D016022:Case-Control Studies; D002851:Chromatography, High Pressure Liquid / Q000379:methods* / Q000592:standards; D056148:Chromatography, Reverse-Phase / Q000379:methods* / Q000592:standards; D006197:Hair / Q000737:chemistry*; D006213:Hallucinogens / Q000032:analysis*; D006801:Humans; D006863:Hydrogen-Ion Concentration; D057230:Limit of Detection; D016014:Linear Models; D008297:Male; D028321:Plant Preparations / Q000032:analysis*; D012015:Reference Standards; D015203:Reproducibility of Results; D012997:Solvents / Q000737:chemistry; D021241:Spectrometry, Mass, Electrospray Ionization / Q000592:standards; D015813:Substance Abuse Detection / Q000379:methods* / Q000592:standards; D019966:Substance-Related Disorders / Q000175:diagnosis*; D053719:Tandem Mass Spectrometry / Q000592:standards
chemical_list: D002021:Buffers; D006213:Hallucinogens; D028321:Plant Preparations; D012997:Solvents
keywords: Hair testing; Mescaline; N,N-dimethyltriptamine; Psilocin; Salvinorin A; UHPLC–MS/MS