期刊
FORENSIC SCIENCE INTERNATIONAL
卷 312, 期 -, 页码 -出版社
ELSEVIER IRELAND LTD
DOI: 10.1016/j.forsciint.2020.110304
关键词
Seized drugs; New psychoactive substances; Illicit stimulants; Reference standard; Nitrogen chemiluminescence detection; Time-of-flight mass spectrometry
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 alpha-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. (C) 2020 Elsevier B.V. All rights reserved.
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