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Multi‐class analysis of new psychoactive substances and metabolites in hair by pressurized liquid extraction coupled to HPLC‐HRMS
Author(s) -
Montesano Camilla,
Vannutelli Gabriele,
Massa Maristella,
Simeoni Maria Chiara,
Gregori Adolfo,
Ripani Luigi,
Compag Dario,
Curini Roberta,
Sergi Manuel
Publication year - 2017
Publication title -
drug testing and analysis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.065
H-Index - 54
eISSN - 1942-7611
pISSN - 1942-7603
DOI - 10.1002/dta.2043
Subject(s) - chromatography , hair analysis , chemistry , designer drug , extraction (chemistry) , synthetic cannabinoids , solid phase extraction , forensic toxicology , analyte , detection limit , mass spectrometry , high performance liquid chromatography , liquid chromatography–mass spectrometry , drug , pharmacology , cannabinoid , medicine , biochemistry , alternative medicine , receptor , pathology
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 ‐1 for cathinones, phenetylamines and piperazines, and from 9 to 40 pg mg ‐1 for synthetic cannabinoids (10 pg mg ‐1 for 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.