Fast HPLC-MS/MS screening method for identification of illegal drugs including new psychoactive substances and their metabolites in human urine

2020 ◽  
Vol 63 (2) ◽  
pp. 32
Author(s):  
S.A. Savchuk ◽  
K.M. Shestakova ◽  
L.N. Rizvanova ◽  
D.A. Burmykin ◽  
M.V. Ovcharov ◽  
...  
2020 ◽  
Vol 44 (7) ◽  
pp. 697-707
Author(s):  
Kelly Francisco da Cunha ◽  
Karina Diniz Oliveira ◽  
Marilyn A Huestis ◽  
Jose Luiz Costa

Abstract New psychoactive substances (NPS) are a major public health problem, primarily due to the increased number of acute poisoning cases. Detection of these substances is a challenge. The aim of this research was to develop and validate a sensitive screening method for 104 drugs of abuse, including synthetic cannabinoids, synthetic cathinones, fentanyl analogues, phenethylamines and other abused psychoactive compounds (i.e., THC, MDMA, LSD and their metabolites) in oral fluid by liquid chromatography–tandem mass spectrometry (LC–MS-MS). The Quantisal™ oral fluid device was used to collect oral fluid samples. The oral fluid–elution buffer mixture (500-μL sample) was extracted with t-butyl methyl ether, and chromatographic separation was performed on a Raptor™ biphenyl column (100 × 2.1 mm ID, 2.7 μm), with a total run time of 13.5 min. Limits of detection were established at three concentrations (0.05, 0.1 or 1 ng/mL) for most analytes, except for acetyl norfentanyl and mescaline (5 ng/mL). Matrix effects were generally <20% and overall extraction recoveries >60%. The highest matrix effect was observed within the synthetic cannabinoid group (PB22, −55.5%). Lower recoveries were observed for 2C-T (47.2%) and JWH-175 (58.7%). Recoveries from the Quantisal™ device were also evaluated for all analytes (56.7–127%), with lower recoveries noted for 25I-NBOMe, valerylfentanyl and mCPP (56.7, 63.0 and 69.9%, respectively). Drug stability in oral fluid was evaluated at 15, 60 and 90 days and at 25, 4 and −20°C. As expected, greater stability was observed when samples were stored at −20°C, but even when frozen, some NPS (e.g., synthetic cannabinoids) showed more than 20% degradation. The method was successfully applied to the analysis of seven authentic oral fluid samples positive for 17 different analytes. The method achieved good sensitivity and simultaneous detection of a wide range of NPS.


2020 ◽  
Vol 10 (1) ◽  
Author(s):  
Anna Maria Sulej-Suchomska ◽  
Agnieszka Klupczynska ◽  
Paweł Dereziński ◽  
Jan Matysiak ◽  
Piotr Przybyłowski ◽  
...  

2021 ◽  
Vol 19 (1) ◽  
pp. 60-106
Author(s):  
Vera Lukić ◽  
Ružica Micić ◽  
Biljana Arsić ◽  
Bojan Nedović ◽  
Živana Radosavljević

Abstract The misuse of psychoactive substances is attracting a great deal of attention from the general public. An increase use of psychoactive substances is observed among young people who do not have enough awareness of the harmful effects of these substances. Easy access to illicit drugs at low cost and lack of effective means of routine screening for new psychoactive substances (NPS) have contributed to the rapid increase in their use. New research and evidence suggest that drug use can cause a variety of adverse psychological and physiological effects on human health (anxiety, panic, paranoia, psychosis, and seizures). We describe different classes of these NPS drugs with emphasis on the methods used to identify them and the identification of their metabolites in biological specimens. This is the first review that thoroughly gives the literature on both natural and synthetic illegal drugs with old known data and very hot new topics and investigations, which enables the researcher to use it as a starting point in the literature exploration and planning of the own research. For the first time, the conformational analysis was done for selected illegal drugs, giving rise to the search of the biologically active conformations both theoretically and using lab experiments.


2019 ◽  
Vol 16 (33) ◽  
pp. 206-224
Author(s):  
K. M. SHESTAKOVA ◽  
S. A. SAVCHUK ◽  
N. V. MESONZHNIK ◽  
A. V. KUHARENKO ◽  
S. A. APPOLONOVA

The ongoing appearance of new psychoactive substances on the black market of illegal drugs, as well as the lack of information on their influence on the human body, faces several challenges in their determination by standard analytical techniques. Moreover, the rapid metabolism of new psychoactive substances reveals in the absence of possibility in the identification of their native structures in biological fluids. This study presents a new screening method for determination 137 psychoactive substances including their metabolites. 'Dilute-and-shoot' method was chosen as the preferable sample preparation technique, and consisted of 1:5 dilution of urine specimens with the solution of acetonitrile and water (30:70) followed by electrospray ionization – liquid chromatography-tandem mass spectrometry analysis. The developed qualitative method was validated according to United Nations Office on Drugs and Crime requirements that included assessment of selectivity, limits of detection, precision, and stability. In addition, the presented method was tested on 50 certified positive urine specimens containing different drugs of abuse. The confirmatory analysis was performed using a high-resolution mass-spectrometry approach. The presented screening method provides the possibility of simultaneous determination of synthetic cannabinoids (96), opioid analgesics (16), stimulators (13), hallucinogens (5), benzodiazepines (5) and non-classified drugs (10) during one run. The validation assessments of the novel method have shown high rates of its specificity, selectivity, intra- and inter-day precision and stability with the limit of detection ranged from 1 to 5 ng?mL-1. At the same time, tests of 50 positive samples showed excellent applicability of the developed screening method for routine preliminary screening analysis in toxicological laboratories.


2016 ◽  
Vol 129 ◽  
pp. 441-449 ◽  
Author(s):  
Fabio Vaiano ◽  
Francesco P. Busardò ◽  
Diego Palumbo ◽  
Chrystalla Kyriakou ◽  
Alessia Fioravanti ◽  
...  

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