title: Multi-class analysis of new psychoactive substances and metabolites in hair by pressurized liquid extraction coupled to HPLC-HRMS.
abstract: In this paper, an analytical method has been developed and validated for the analysis of new psychoactive substances (NPS) and metabolites in hair samples. The method was based on pressurized liquid extraction (PLE) followed by solid-phase extraction (SPE) clean-up and high performance liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) analysis. To evaluate extraction efficiency and the applicability of the method, hair samples were fortified by soaking in order to obtain a good surrogate for drug users' hair; the amount of incorporated drugs related to their lipophilicity, similarly to in vivo drug incorporation. To the best of our knowledge, this is the first method that allowed for the analysis of both cathinones (5) and synthetic cannabinoids (7) in hair with a single extraction procedure and chromatographic run. A phenethylamine (2C-T-4), 4- fluorophenylpiperazine and methoxetamine were also included showing that PLE coupled to SPE clean-up was suitable for a multi-class analysis of NPS in hair. In addition, the use of PLE significantly reduced hair analysis time: decontamination, incubation, clean-up, and liquid chromatography-mass spectrometry (LC-MS) analysis were carried out in approximately 45 min. The method was fully validated according to Scientific Working Group for Forensic Toxicology (SWGTOX) and Society of Hair Testing (SoHT) guidelines. Limit of quantification (LOQ) values ranged from 8 to 50 pg mg-1for cathinones, phenetylamines and piperazines, and from 9 to 40 pg mg-1for synthetic cannabinoids (10 pg mg-1for methoxetamine). Matrix effects were below 15% for all the analytes, demonstrating the effectiveness of the clean-up step. Inaccuracy was lower than 9% in terms of bias. Copyright © 2016 John Wiley & Sons, Ltd.
authors.affiliation: Department of Chemistry, Sapienza University of Rome, 00185, Rome, Italy.
authors.forename: Camilla
authors.initials: C
authors.lastname: Montesano
authors.affiliation: Department of Chemistry, Sapienza University of Rome, 00185, Rome, Italy.
authors.forename: Gabriele
authors.initials: G
authors.lastname: Vannutelli
authors.affiliation: Department of Chemistry, Sapienza University of Rome, 00185, Rome, Italy.
authors.forename: Maristella
authors.initials: M
authors.lastname: Massa
authors.affiliation: Faculty of Bioscience and Technology for Food, Agriculture and Environment, University of Teramo, 64023, Mosciano Sant'Angelo, TE, Italy.
authors.forename: Maria Chiara
authors.initials: MC
authors.lastname: Simeoni
authors.affiliation: Department of Scientific Investigation (RIS), Carabinieri, 00191, Rome, Italy.
authors.forename: Adolfo
authors.initials: A
authors.lastname: Gregori
authors.affiliation: Department of Scientific Investigation (RIS), Carabinieri, 00191, Rome, Italy.
authors.forename: Luigi
authors.initials: L
authors.lastname: Ripani
authors.affiliation: Faculty of Bioscience and Technology for Food, Agriculture and Environment, University of Teramo, 64023, Mosciano Sant'Angelo, TE, Italy.
authors.forename: Dario
authors.initials: D
authors.lastname: Compagnone
authors.affiliation: Department of Chemistry, Sapienza University of Rome, 00185, Rome, Italy.
authors.forename: Roberta
authors.initials: R
authors.lastname: Curini
authors.affiliation: Faculty of Bioscience and Technology for Food, Agriculture and Environment, University of Teramo, 64023, Mosciano Sant'Angelo, TE, Italy.
authors.forename: Manuel
authors.initials: M
authors.lastname: Sergi
mesh_terms: D000470:Alkaloids / Q000032:analysis*; D002186:Cannabinoids / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D053593:Forensic Toxicology / Q000379:methods; D006197:Hair / Q000737:chemistry*; D006801:Humans; D013287:Illicit Drugs / Q000032:analysis*; D057230:Limit of Detection; D011619:Psychotropic Drugs / Q000032:analysis*; D052616:Solid Phase Extraction / Q000379:methods; D015813:Substance Abuse Detection / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D000470:Alkaloids; D002186:Cannabinoids; D013287:Illicit Drugs; D011619:Psychotropic Drugs; C023665:cathinone
keywords: HPLC-HRMS; cathinones; hair; new psychoactive substances; synthetic cannabinoids