Determination of 19 Psychoactive Substances in Premortem and Postmortem Whole Blood Samples Using Ultra-High-Performance Liquid Chromatography–Tandem Mass Spectrometry

Abstract

An ever-increasing need exists within the forensic laboratories to develop analytical processes for the qualitative and quantitative determination of a broad spectrum of new psychoactive substances. Phenylethylamine derivatives are among the major classes of psychoactive substances available on the global market and include both amphetamine analogues and synthetic cathinones. In this work, an ultra-high-performance liquid chromatography-positive ion electrospray ionization tandem mass spectrometric method (UHPLC-ESI-MS/MS) has been developed and fully validated for the determination of 19 psychoactive substances, including nine amphetamine-type stimulants and 10 synthetic cathinone derivatives, in premortem and postmortem whole blood. The assay was based on the use of 1 mL premortem or postmortem whole blood, following solid phase extraction prior to the analysis. The separation was achieved on a Poroshell 120 EC-C18 analytical column with a gradient mobile phase of 0.1% formic acid in acetonitrile and 0.1% formic acid in water in 9 min. The dynamic multiple reaction monitoring used in this work allowed for limit of detection (LOD) and lower limit of quantitation (LOQ) values of 0.5 and 2 ng mL−1, respectively, for all analytes both in premortem and postmortem whole blood samples. A quadratic calibration model was used for the 12 quantitative analytes over the concentration range of 20–2000 ng mL−1, and the method was shown to be precise and accurate both in premortem and postmortem whole blood. The method was applied to the analysis of real cases and proved to be a valuable tool in forensic and clinical toxicology.

Interpol Review of Drug Analysis 2019-2022

“…2020 solutions for the selective electrochemical analysis for the detection of cocaine in speedball-like polydrug samples adulterated with heroin and codeine [ 821 ]; review of electrochemical detection of illicit drugs (such as cocaine, heroin, and (meth)amphetamine), their precursors and derivatives in different matrices [ 822 ]; an approach to identify and estimate the purity of white powders as amphetamine, cocaine, ketamine or others using spectroscopic techniques hyphenated with partial least squares (PLS) modelling [ 823 ]; electron ionization (EI) and electrospray ionization (ESI) high-resolution mass spectrometry fragmentation pathways and characteristic ions of 25 novel fentanyl analogues and 5 novel synthetic opioids to provide a reference for the identification of these compounds [ 651 ]; 2021 UHPLC-MS/MS method to determine the designer benzodiazepines (clonazolam, deschloroetizolam, nifoxipam, flubromazolam and meclonazepam), and the Z-hypnotics (zolpidem, zaleplon and zopiclone) [ 824 ]; an ultrasonic cutter-assisted non-thermal desorption (non-TD) method for ultra-trace level detection of different types of nonvolatile compounds such as drugs of abuse, explosives, pharmaceuticals, spinosad, cholesterol, rhodamine B, glucose and amino acids [ 825 ]; HR-EIS-QTOF-MS comparison study of in-source versus beam-type collision-induced dissociation for fentanyl analogues and synthetic cathinones [ 826 ]; ATR-FTIR method used with PCA, Fisher discriminant analysis (FDA), and K nearest neighbor analysis (KNN) to develop a method for differentiating barbiturates, benzodiazepines, and phenothiazines [ 827 ]; H-1 and F-19 NMR spectroscopy method for the dection, discrimination and quantification of amphetamine, cathinone and nor-ephedrine regioisomers [ 828 ]; validated UHPLC-ESI-MS/MS method for determination of 19 psychoactive substances, including nine amphetamine-type stimulants and 10 synthetic cathinone derivatives [ 829 ]; review of the research on chiral separation of amphetamines, ketamine, cathinones [ 830 ]; 2022 Comparison of two seized drug workflows for the analysis of synthetic cannabinoids, cathinones, and opioids that includes color tests for screening with GC-FID and GC-MS analyses for confirmation verus DART-MS screening with class-specific (targeted) GC-MS [ 831 ].…”