Targeted and untargeted detection of fentanyl analogues and their metabolites in hair by means of UHPLC-QTOF-HRMS
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RESEARCH PAPER
Targeted and untargeted detection of fentanyl analogues and their metabolites in hair by means of UHPLC-QTOF-HRMS Alberto Salomone 1,2 Marco Vincenti 1,2
&
Daniele Di Corcia 1 & Pierre Negri 3 & Maria Kolia 4 & Eleonora Amante 2 & Enrico Gerace 1 &
Received: 27 July 2020 / Revised: 25 September 2020 / Accepted: 6 October 2020 # The Author(s) 2020
Abstract Detection of new psychoactive substances and synthetic opioids is generally performed by means of targeted methods in mass spectrometry, as they generally provide adequate sensitivity and specificity. Unfortunately, new and unexpected compounds are continuously introduced in the illegal market of abused drugs, preventing timely updating of the analytical procedures. Moreover, the investigation of biological matrices is influenced by metabolism and excretion, in turn affecting the chance of past intake detectability. In this scenario, new opportunities are offered by both the non-targeted approaches allowed by modern UHPLCHRMS instrumentation and the investigation of hair as the matrix of choice to detect long-term exposure to toxicologically relevant substances. In this study, we present a comprehensive and validated workflow that combines the use of UHPLC-QTOFHRMS instrumentation with a simple hair sample extraction procedure for the detection of a variety of fentanyl analogues and metabolites. A simultaneous targeted and untargeted analysis was applied to 100 real samples taken from opiates users. MS and MS/MS data were collected for each sample. Data acquisition included a TOF-MS high-resolution scan combined with TOF-MS/ MS acquisition demonstrating considerable capability to detect expected and unexpected substances even at low concentration levels. The predominant diffusion of fentanyl was confirmed by its detection in 68 hair samples. Other prevalent analogues were furanylfentanyl (28 positive samples) and acetylfentanyl (14 positive samples). Carfentanil, methylfentanyl, and ocfentanil were not found in any of the analyzed samples. Furthermore, the retrospective data analysis based on untargeted acquisition allowed the identification of two fentanyl analogues, namely β-hydroxyfentanyl and methoxyacetylfentanyl, which were not originally included in the panel of targeted analytes. Keywords Hair . NPS . QTOF . NSO . SWATH . Fentanyl . Untargeted
Introduction Electronic supplementary material The online version of this article (https://doi.org/10.1007/s00216-020-02994-x) contains supplementary material, which is available to authorized users. * Alberto Salomone [email protected] 1
Centro Regionale Antidoping e di Tossicologia, Regione Gonzole 10/1, 10043 Orbassano, TO, Italy
2
Department of Chemistry, University of Turin, Via Pietro Giuria 5, 10125 Torino, Italy
3
AB SCIEX, Redwood City, CA 01701, USA
4
Department of Chemistry, University of Ioannina, Ioannina Campus, 1186, Ioannina 45500, Greece
In the last decade, the general situation and world distribution of drugs of abuse has evolved dramatically with the emergence o
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