New screening and quantification method by UHPLC-MS/MS of 36 new synthetic cathinones in hair. Application to real cases

A class of β-keto analogs of phenethylamine known as synthetic cathinones has been identified as the most emergent new class of psychoactive chemicals in the last ten years. Synthetic cathinones (SC) are becoming more varied, which represents a serious danger to social security and public health wor...

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Main Authors: Alfredo Fabrizio Lo Faro, Anastasio Tini, Giorgi Kobidze, Giulio Mannocchi, Massimo Gottardi, Francesco Paolo Busardò, Giuseppe Basile, Bezhan Chakvetadze
Format: Article
Language:English
Published: Elsevier 2024-12-01
Series:Journal of Pharmaceutical and Biomedical Analysis Open
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Online Access:http://www.sciencedirect.com/science/article/pii/S2949771X24000161
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author Alfredo Fabrizio Lo Faro
Anastasio Tini
Giorgi Kobidze
Giulio Mannocchi
Massimo Gottardi
Francesco Paolo Busardò
Giuseppe Basile
Bezhan Chakvetadze
author_facet Alfredo Fabrizio Lo Faro
Anastasio Tini
Giorgi Kobidze
Giulio Mannocchi
Massimo Gottardi
Francesco Paolo Busardò
Giuseppe Basile
Bezhan Chakvetadze
author_sort Alfredo Fabrizio Lo Faro
collection DOAJ
description A class of β-keto analogs of phenethylamine known as synthetic cathinones has been identified as the most emergent new class of psychoactive chemicals in the last ten years. Synthetic cathinones (SC) are becoming more varied, which represents a serious danger to social security and public health worldwide. In this work, an analytical technique based on UHPLC-MS/MS was developed for the simultaneously measurement of 36 synthetic cathinones and two metabolites in hair keratin samples. The separation was conducted by Atlantis Premier BEH C18 AX (2.5 μm, 2.1 × 100 mm) column using elution with 5 mM ammonium acetate in water with 0.1 % formic acid (v/v) (mobile phase A) and 2 mM ammonium formate in MeOH/Acetonitrile 50/50, +0.1 % formic acid (v/v) (mobile phase B). The analysis time was 11 min. Mass spectrometer was equipped with electrospray ionization (ESI). Multiple reaction monitoring (MRM) mode was used for the detection and quantification of the studied compounds. The methodology was successfully validated according to the Organization Scientific Area Committee guidelines, with linearity (r2 ≥ 0.99) from LOQ to 500 pg/mg concentrations for all the compounds investigated. This method was subsequently applied to nine hair samples positive for ten different synthetic cathinones. The most common SCs identified were 3,4-methylenedioxypyrovalerone (3,4-MDPV), in a concentration range 6.0–1000.0 pg/mg, along with alpha-pyrrolidinopentiophenone (α-PHP (54.0 and 554.0 pg/mg, respectively)), followed by the two positional isomers 3-MMC (556.0 and 5000.0 pg/mg) and 4-MMC (11.5 and 448.0 pg/mg). In conclusion, a validated LC-MS/MS method with high specificity was developed offering an easy and affordable sample preparation, and a run time that makes it suitable for use in a high throughput forensic laboratory for the multi-analyte quantification of 36 novel synthetic cathinones and 2 metabolites in hair.
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spelling doaj-art-889380bd1f5e446186b72e580fb07af02025-08-20T02:51:38ZengElsevierJournal of Pharmaceutical and Biomedical Analysis Open2949-771X2024-12-01410004010.1016/j.jpbao.2024.100040New screening and quantification method by UHPLC-MS/MS of 36 new synthetic cathinones in hair. Application to real casesAlfredo Fabrizio Lo Faro0Anastasio Tini1Giorgi Kobidze2Giulio Mannocchi3Massimo Gottardi4Francesco Paolo Busardò5Giuseppe Basile6Bezhan Chakvetadze7Department of Excellence-Biomedical Sciences and Public Health, Università Politecnica delle Marche, Ancona 60121, ItalyDepartment of Excellence-Biomedical Sciences and Public Health, Università Politecnica delle Marche, Ancona 60121, ItalyDepartment of Excellence-Biomedical Sciences and Public Health, Università Politecnica delle Marche, Ancona 60121, ItalyComedical S.r.l, Trento 38123, ItalyComedical S.r.l, Trento 38123, ItalyDepartment of Excellence-Biomedical Sciences and Public Health, Università Politecnica delle Marche, Ancona 60121, Italy; Corresponding author.Department of Trauma Surgery, IRCCS Galeazzi Orthopedic Institute, Milan, ItalyInstitute of Physical and Analytical Chemistry, School of Exact and Natural Sciences, Tbilisi State University, I. Chavchavadze Ave 1, Tbilisi 0179, GeorgiaA class of β-keto analogs of phenethylamine known as synthetic cathinones has been identified as the most emergent new class of psychoactive chemicals in the last ten years. Synthetic cathinones (SC) are becoming more varied, which represents a serious danger to social security and public health worldwide. In this work, an analytical technique based on UHPLC-MS/MS was developed for the simultaneously measurement of 36 synthetic cathinones and two metabolites in hair keratin samples. The separation was conducted by Atlantis Premier BEH C18 AX (2.5 μm, 2.1 × 100 mm) column using elution with 5 mM ammonium acetate in water with 0.1 % formic acid (v/v) (mobile phase A) and 2 mM ammonium formate in MeOH/Acetonitrile 50/50, +0.1 % formic acid (v/v) (mobile phase B). The analysis time was 11 min. Mass spectrometer was equipped with electrospray ionization (ESI). Multiple reaction monitoring (MRM) mode was used for the detection and quantification of the studied compounds. The methodology was successfully validated according to the Organization Scientific Area Committee guidelines, with linearity (r2 ≥ 0.99) from LOQ to 500 pg/mg concentrations for all the compounds investigated. This method was subsequently applied to nine hair samples positive for ten different synthetic cathinones. The most common SCs identified were 3,4-methylenedioxypyrovalerone (3,4-MDPV), in a concentration range 6.0–1000.0 pg/mg, along with alpha-pyrrolidinopentiophenone (α-PHP (54.0 and 554.0 pg/mg, respectively)), followed by the two positional isomers 3-MMC (556.0 and 5000.0 pg/mg) and 4-MMC (11.5 and 448.0 pg/mg). In conclusion, a validated LC-MS/MS method with high specificity was developed offering an easy and affordable sample preparation, and a run time that makes it suitable for use in a high throughput forensic laboratory for the multi-analyte quantification of 36 novel synthetic cathinones and 2 metabolites in hair.http://www.sciencedirect.com/science/article/pii/S2949771X24000161Synthetic cathinonesHairUHPLC-MS/MSNew Psychoactive Substances
spellingShingle Alfredo Fabrizio Lo Faro
Anastasio Tini
Giorgi Kobidze
Giulio Mannocchi
Massimo Gottardi
Francesco Paolo Busardò
Giuseppe Basile
Bezhan Chakvetadze
New screening and quantification method by UHPLC-MS/MS of 36 new synthetic cathinones in hair. Application to real cases
Journal of Pharmaceutical and Biomedical Analysis Open
Synthetic cathinones
Hair
UHPLC-MS/MS
New Psychoactive Substances
title New screening and quantification method by UHPLC-MS/MS of 36 new synthetic cathinones in hair. Application to real cases
title_full New screening and quantification method by UHPLC-MS/MS of 36 new synthetic cathinones in hair. Application to real cases
title_fullStr New screening and quantification method by UHPLC-MS/MS of 36 new synthetic cathinones in hair. Application to real cases
title_full_unstemmed New screening and quantification method by UHPLC-MS/MS of 36 new synthetic cathinones in hair. Application to real cases
title_short New screening and quantification method by UHPLC-MS/MS of 36 new synthetic cathinones in hair. Application to real cases
title_sort new screening and quantification method by uhplc ms ms of 36 new synthetic cathinones in hair application to real cases
topic Synthetic cathinones
Hair
UHPLC-MS/MS
New Psychoactive Substances
url http://www.sciencedirect.com/science/article/pii/S2949771X24000161
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