Application of Fabric Phase Sorptive Extraction (FPSE) Engaged to Tandem LC-MS/MS for Quantification of Brorphine in Oral Fluid

Brorphine (1-[1-[1-(4-bromophenyl) ethyl]-piperidin-4-yl]-1,3-dihydro-2H-benzo [d]imidazol-2-one) is one of the most recent novel synthetic opioids (NSOs) on the novel psychoactive substances (NPSs) market, involved in over 100 deaths in 2020. Brorphine is a substituted piperidine-benzimidazolone an...

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Main Authors: Dimitra Florou, Thalia Vlachou, Vasilios Sakkas, Vassiliki Boumba
Format: Article
Language:English
Published: MDPI AG 2022-11-01
Series:Journal of Xenobiotics
Subjects:
Online Access:https://www.mdpi.com/2039-4713/12/4/25
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author Dimitra Florou
Thalia Vlachou
Vasilios Sakkas
Vassiliki Boumba
author_facet Dimitra Florou
Thalia Vlachou
Vasilios Sakkas
Vassiliki Boumba
author_sort Dimitra Florou
collection DOAJ
description Brorphine (1-[1-[1-(4-bromophenyl) ethyl]-piperidin-4-yl]-1,3-dihydro-2H-benzo [d]imidazol-2-one) is one of the most recent novel synthetic opioids (NSOs) on the novel psychoactive substances (NPSs) market, involved in over 100 deaths in 2020. Brorphine is a substituted piperidine-benzimidazolone analogue that retains structural similarities to fentanyl, acting as a full agonist at the μ-opioid receptor. Oral Fluid (OF) is an alternative matrix, frequently analyzed for the detection of NPS. Fabric phase sorptive extraction (FPSE) is a superior, green-sample -preparation technology recently applied for drug analysis. This contribution presents the development and validation of a method, based on the application of FPSE and liquid chromatography–tandem mass spectrometry (LC-MS/MS), to determine/quantitate brorphine in OF. The method’s linearity ranged between 0.05 and 50 ng/mL (R<sup>2</sup> = 0.9993), the bias ranged between 12.0 and 16.8%, and inter- and intra-day precisions ranged between 6.4 and 9.9%. Accuracy and extraction efficiency lied between 65 and 75%. LOD/LOQ were 0.015 ng/mL/0.05 ng/mL. Analyte’s post-preparative stability was higher than 95%, while no matrix interferences and carryover between runs were observed. This is the first report introducing the application of FPSE for NPS determination, specifically, the quantification of brorphine in OF, thereby presenting a simple, rapid, sensitive, specific, effective, and reliable procedure engaged to LC-MS/MS that is suitable for routine application and the analysis of more NPSs.
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spelling doaj.art-7c38b111a7dc427dbbfec15c31b0b2282023-11-24T16:00:48ZengMDPI AGJournal of Xenobiotics2039-47052039-47132022-11-0112435636410.3390/jox12040025Application of Fabric Phase Sorptive Extraction (FPSE) Engaged to Tandem LC-MS/MS for Quantification of Brorphine in Oral FluidDimitra Florou0Thalia Vlachou1Vasilios Sakkas2Vassiliki Boumba3Department of Forensic Medicine and Toxicology, Faculty of Medicine, School of Health Sciences, University of Ioannina, University Campus, 5110 Ioannina, GreeceDepartment of Forensic Medicine and Toxicology, Faculty of Medicine, School of Health Sciences, University of Ioannina, University Campus, 5110 Ioannina, GreeceDepartment of Analytical Chemistry, Faculty of Chemistry, University of Ioannina, 5110 Ioannina, GreeceDepartment of Forensic Medicine and Toxicology, Faculty of Medicine, School of Health Sciences, University of Ioannina, University Campus, 5110 Ioannina, GreeceBrorphine (1-[1-[1-(4-bromophenyl) ethyl]-piperidin-4-yl]-1,3-dihydro-2H-benzo [d]imidazol-2-one) is one of the most recent novel synthetic opioids (NSOs) on the novel psychoactive substances (NPSs) market, involved in over 100 deaths in 2020. Brorphine is a substituted piperidine-benzimidazolone analogue that retains structural similarities to fentanyl, acting as a full agonist at the μ-opioid receptor. Oral Fluid (OF) is an alternative matrix, frequently analyzed for the detection of NPS. Fabric phase sorptive extraction (FPSE) is a superior, green-sample -preparation technology recently applied for drug analysis. This contribution presents the development and validation of a method, based on the application of FPSE and liquid chromatography–tandem mass spectrometry (LC-MS/MS), to determine/quantitate brorphine in OF. The method’s linearity ranged between 0.05 and 50 ng/mL (R<sup>2</sup> = 0.9993), the bias ranged between 12.0 and 16.8%, and inter- and intra-day precisions ranged between 6.4 and 9.9%. Accuracy and extraction efficiency lied between 65 and 75%. LOD/LOQ were 0.015 ng/mL/0.05 ng/mL. Analyte’s post-preparative stability was higher than 95%, while no matrix interferences and carryover between runs were observed. This is the first report introducing the application of FPSE for NPS determination, specifically, the quantification of brorphine in OF, thereby presenting a simple, rapid, sensitive, specific, effective, and reliable procedure engaged to LC-MS/MS that is suitable for routine application and the analysis of more NPSs.https://www.mdpi.com/2039-4713/12/4/25brorphineFPSELC-MS/MSNPSNSOoral fluid
spellingShingle Dimitra Florou
Thalia Vlachou
Vasilios Sakkas
Vassiliki Boumba
Application of Fabric Phase Sorptive Extraction (FPSE) Engaged to Tandem LC-MS/MS for Quantification of Brorphine in Oral Fluid
Journal of Xenobiotics
brorphine
FPSE
LC-MS/MS
NPS
NSO
oral fluid
title Application of Fabric Phase Sorptive Extraction (FPSE) Engaged to Tandem LC-MS/MS for Quantification of Brorphine in Oral Fluid
title_full Application of Fabric Phase Sorptive Extraction (FPSE) Engaged to Tandem LC-MS/MS for Quantification of Brorphine in Oral Fluid
title_fullStr Application of Fabric Phase Sorptive Extraction (FPSE) Engaged to Tandem LC-MS/MS for Quantification of Brorphine in Oral Fluid
title_full_unstemmed Application of Fabric Phase Sorptive Extraction (FPSE) Engaged to Tandem LC-MS/MS for Quantification of Brorphine in Oral Fluid
title_short Application of Fabric Phase Sorptive Extraction (FPSE) Engaged to Tandem LC-MS/MS for Quantification of Brorphine in Oral Fluid
title_sort application of fabric phase sorptive extraction fpse engaged to tandem lc ms ms for quantification of brorphine in oral fluid
topic brorphine
FPSE
LC-MS/MS
NPS
NSO
oral fluid
url https://www.mdpi.com/2039-4713/12/4/25
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AT vasiliossakkas applicationoffabricphasesorptiveextractionfpseengagedtotandemlcmsmsforquantificationofbrorphineinoralfluid
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