scholarly journals Guilty by dissociation—development of gas chromatography–mass spectrometry (GC-MS) and other rapid screening methods for the analysis of 13 diphenidine-derived new psychoactive substances (NPSs)

2016 ◽  
Vol 408 (29) ◽  
pp. 8467-8481 ◽  
Author(s):  
Pierre M. Geyer ◽  
Matthew C. Hulme ◽  
Joseph P. B. Irving ◽  
Paul D. Thompson ◽  
Ryan N. Ashton ◽  
...  
2017 ◽  
Vol 9 (18) ◽  
pp. 2732-2743 ◽  
Author(s):  
Khalid A. Alsenedi ◽  
Calum Morrison

Insight into mass spectrometry ions and derivatization conditions for synthetic cathinone type new psychoactive substances.


Author(s):  
Margalho Cláudia ◽  
Almeida Pedro ◽  
Rosado Tiago ◽  
Corte Real Francisco ◽  
Gallardo Eugenia

Abstract The production and consumption of new psychoactive substances (NPSs) has been raising a major concern worldwide. Due to easy access and available information, many NPSs continue to be synthesized with an alarming increase of those available to purchase, despite all the control efforts created. A new analytical method was developed and validated to determine a group of phenethylamines and synthetic cathinones: cathinone, flephedrone, buphedrone, 4-MTA, α-PVP, methylone, 2C-P, ethylone, pentylone, MDPV and bromo-dragonFLY in whole blood. A mixed-mode solid phase extraction was applied to 250 μL of sample, and the extracts were derivatized with fast microwave technique before being analyzed by gas chromatography–mass spectrometry (GC–MS). The validation procedure followed the Scientific Working Group for Forensic Toxicology (SWGTOX) guidelines with parameters that included selectivity, linearity, limits of detection and quantification, intra- and inter-day precision and accuracy, recoveries and stability. The method presented linearity between 5 and 500 ng/mL for cathinone, buphedrone, 4-MTA, methylone, 2C-P and bromo-dragonFLY, 10–500 ng/mL for flephedrone, ethylone, pentylone and MDPV, and 40–500 ng/mL for α-PVP, with determination coefficients above 0.99 for all analytes. Recoveries ranged between 70.3% and 116.6%, and regarding intra- and inter-day precision, the relative mean errors were typically lower than 8.6%. The method was successfully applied to over 100 authentic samples from the Laboratory of Chemistry and Forensic Toxicology, Centre Branch, of the National Institute of Legal Medicine and Forensic Sciences, Portugal.


2021 ◽  
Vol 22 (8) ◽  
pp. 4000
Author(s):  
Emilia Marchei ◽  
Maria Alias Ferri ◽  
Marta Torrens ◽  
Magí Farré ◽  
Roberta Pacifici ◽  
...  

The use of the new psychoactive substances is continuously growing and the implementation of accurate and sensible analysis in biological matrices of users is relevant and fundamental for clinical and forensic purposes. Two different analytical technologies, high-sensitivity gas chromatography-mass spectrometry (GC-MS) and ultra-high-performance liquid chromatography-high-resolution mass spectrometry (UHPLC-HRMS) were used for a screening analysis of classic drugs and new psychoactive substances and their metabolites in urine of formed heroin addicts under methadone maintenance therapy. Sample preparation involved a liquid-liquid extraction. The UHPLC-HRMS method included Accucore™ phenyl Hexyl (100 × 2.1 mm, 2.6 μm, Thermo, USA) column with a gradient mobile phase consisting of mobile phase A (ammonium formate 2 mM in water, 0.1% formic acid) and mobile phase B (ammonium formate 2 mM in methanol/acetonitrile 50:50 (v/v), 0.1% formic acid) and a full-scan data-dependent MS2 (ddMS2) mode for substances identification (mass range 100–1000 m/z). The GC-MS method employed an ultra-Inert Intuvo GC column (HP-5MS UI, 30 m, 250 µm i.d, film thickness 0.25 µm; Agilent Technologies, Santa Clara, CA, USA) and electron-impact (EI) mass spectra were recorded in total ion monitoring mode (scan range 40–550 m/z). Urine samples from 296 patients with a history of opioid use disorder were examined. Around 80 different psychoactive substances and/or metabolites were identified, being methadone and metabolites the most prevalent ones. The possibility to screen for a huge number of psychotropic substances can be useful in suspected drug related fatalities or acute intoxication/exposure occurring in emergency departments and drug addiction services.


2019 ◽  
Vol 1125 ◽  
pp. 121731 ◽  
Author(s):  
Ricardo Gonçalves ◽  
Cláudia Ribeiro ◽  
Sara Cravo ◽  
Sara C. Cunha ◽  
José Augusto Pereira ◽  
...  

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