Purity estimation of seized stimulant-type new psychoactive substances without reference standards by nitrogen chemiluminescence detection combined with GC-APCI-QTOFMS

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Mesihää , S , Rasanen , I & Ojanperä , I 2020 , ' Purity estimation of seized stimulant-type new psychoactive substances without reference standards by nitrogen chemiluminescence detection combined with GC-APCI-QTOFMS ' , Forensic Science International , vol. 312 , 110304 . https://doi.org/10.1016/j.forsciint.2020.110304

Title: Purity estimation of seized stimulant-type new psychoactive substances without reference standards by nitrogen chemiluminescence detection combined with GC-APCI-QTOFMS
Author: Mesihää, Samuel; Rasanen, Ilpo; Ojanperä, Ilkka
Contributor: University of Helsinki, Department of Forensic Medicine
University of Helsinki, Department of Forensic Medicine
Date: 2020-07
Language: eng
Number of pages: 6
Belongs to series: Forensic Science International
ISSN: 0379-0738
URI: http://hdl.handle.net/10138/329505
Abstract: Purity assessment of seized material containing new psychoactive substances (NPS) is complicated without appropriate primary reference standards. Here we present a method for fast quantitative estimation of stimulant-type NPS with use of secondary reference standards, based on gas chromatography nitrogen chemiluminescence detection coupled with atmospheric pressure chemical ionization quadrupole time-of-flight mass spectrometry (GC-NCD-APCI-QTOFMS). Quantification was based on the detector’s N-equimolar response to nitrogen and using two external nitrogen-containing calibrators, MDMA for prim- and sec- amines and α-PVP for tert- amines. Sample preparation involved dissolving the seized powdery material in an organic solvent mixture followed by acylation with N-methyl-bis-trifluoroacetamide (MBTFA). The method’s between-day accuracy and precision over a five-day period was measured for twenty-eight stimulants: the grand mean equimolarity was 91.9% (CV 5.5%), as compared with primary reference standards. The GC-NCD-APCI-QTOFMS method was applied to the purity estimation of forty-two seized powder samples previously found to contain stimulant-type NPS by appropriate methods. The quantitative results were compared to those obtained by an established method relying on liquid chromatography chemiluminescence detection (LC-CLND), the latter using caffeine as an external calibrator. The mean difference of purity values between the methods was 8.1% (range 0.4 - 26.7%). The presented method might find use as a tool for instant purity assessment in forensic laboratories.
Subject: Seized drugs
New psychoactive substances
Illicit stimulants
Reference standard
Nitrogen chemiluminescence detection
Time-of-flight mass spectrometry
METABOLITES
LIQUID-CHROMATOGRAPHY
QUANTITATIVE NMR
QUANTIFICATION
ABSENCE
IDENTIFICATION
319 Forensic science and other medical sciences
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