scholarly journals DEVELOPMENT AND APPLICATION OF A RAPID SCREENING METHOD FOR DETERMINATION OF NEW PSYCHOACTIVE SUBSTANCES AND THEIR METABOLITES IN URINE

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.

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):  
Ángela López-Rabuñal ◽  
Daniele Di Corcia ◽  
Eleonora Amante ◽  
Marta Massano ◽  
Angelines Cruz-Landeira ◽  
...  

AbstractNew psychoactive substances (NPS) have been introduced into the market in recent years, with new analytes reported every year. The use of these substances in women can occur at any stage of life, even in the childbearing age. Drug use during pregnancy presents significant risks for the mother and the fetus, so it is important to have tools that allow to detect prenatal exposure to these substances of abuse. Therefore, an analytical method for the determination of 137 NPS and other drugs of abuse in meconium by UHPLC-QTOF was developed and validated for semi-quantitative purpose. Linearity range, limit of detection (LOD), precision, matrix effect, selectivity, and specificity were evaluated. For all analytes, the calibration curves were studied in the ranges between 2, 10, or 50 ng/g and 750 or 1000 ng/g, (depending on the analyte) and the LOD ranged between 0.04 and 2.4 ng/g. The method was applied to 30 meconium specimens from cases in which fentanyl had been administered as epidural anesthesia at the time of delivery or cases in which the maternal hair was positive to other drug of abuse. Four meconium samples tested positive for fentanyl (range concentration = 440–750 ng/g) and two samples tested positive to acetylfentanyl (range concentration = 190–1400 ng/g).


2019 ◽  
Vol 43 (9) ◽  
pp. 734-745 ◽  
Author(s):  
Kristin W Kahl ◽  
Joshua Z Seither ◽  
Lisa J Reidy

Abstract Toxicology laboratories commonly employ immunoassay methodologies to perform an initial drug screen on urine specimens to direct confirmatory testing. Due to limitations of immunoassay testing and the need to screen for a broader range of drugs with lower limits of detection at a lower cost, mass spectrometry screening techniques have gained favor in the toxicology field. A liquid chromatography–tandem mass spectrometry (LC-MS-MS) urine screening panel was developed and validated for 52 drugs and metabolites. A simple dilute-and-shoot with enzymatic hydrolysis technique was utilized to prepare the urine specimens for analysis. Limit of detection, interference, ionization suppression/enhancement, carryover and stability of processed specimens were assessed during validation. To evaluate the toxicological results obtained from utilizing the LC-MS-MS in comparison with the laboratory’s current enzyme-linked immunosorbent assay (ELISA) panel, 100 authentic urine specimens from suspected driving under the influence and drug-facilitated crime cases were analyzed using both methodologies and the results were compared. In addition, the cost of each methodology was evaluated and compared. The validated LC-MS-MS method had limits of detection that were equal to or lower than the concentrations validated for ELISA cutoffs, had fewer exogenous interferences, and the cost of screening per specimen was reduced by ~70% when compared to ELISA. Comparing the toxicology results of forensic urine specimens demonstrated that by only using ELISA, the laboratory was unable to detect benzoylecgonine in 26%, lorazepam in 33% and oxymorphone in 60% of the positive specimens. Additional analytes detected using the LC-MS-MS method were zolpidem and/or metabolite, gabapentin, tramadol and metabolite, methadone and metabolite, meprobamate and phentermine. The results of the validation, the toxicological result comparison and the cost comparison showed that the LC-MS-MS screening method is a simple, sensitive and cost-effective alternative to ELISA screening methods for urine specimens.


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