Development of two fully automated quick, easy, cheap, effective, rugged, and safe pretreatment methods for the extraction of psychotropic drugs from whole blood samples.

Quick, easy, cheap, effective, rugged, and safe extraction strategies are becoming increasingly adopted in various analytical fields to determine drugs in biological specimens. In the present study, we developed two fully automated quick, easy, cheap, effective, rugged, and safe extraction methods based on acetonitrile salting-out assisted liquid-liquid extraction (method 1) and acetonitrile salting-out assisted liquid-liquid extraction followed by dispersive solid-phase extraction (method 2) using a commercially available automated liquid-liquid extraction system. We applied these methods to the extraction of 14 psychotropic drugs (11 benzodiazepines and carbamazepine, quetiapine, and zolpidem) from whole blood samples.

Regioisomer Differentiation of Ring-Substituted Chloromethcathinones and Bromomethcathinones Using Gas Chromatography/Electron Ionization-Triple Quadrupole Energy-Resolved Mass Spectrometry.

Positional isomers -, -, and -chloromethcathinones (CMCs) and - and -bromomethcathinones (BMCs) were effectively differentiated using gas chromatography (GC) and energy-resolved mass spectrometry (ERMS) analyses. GC demonstrated that the free bases of CMC and BMC isomers were simultaneously baseline-separated at a slow column heating rate (5 °C/min) using a conventional low-polar capillary column. ERMS showed that the trifluoroacetyl derivatives of the positional isomers differed in mass spectral abundances of both halophenyl and halobenzoyl cations.

Differentiation of o-, m-, and p-fluoro-α-pyrrolidinopropiophenones by Triton B-mediated one-pot reaction.

Positional isomer differentiation is crucial for the analysis of forensic drugs. Presently, it is difficult to distinguish among ortho, meta, and para positional isomers of ring-fluorinated synthetic cathinones, a major class of new psychoactive substances (NPSs), because they exhibit similar chromatographic properties and mass spectral patterns. We describe herein that the ring-fluorinated synthetic cathinone positional isomers, viz.

Energy-resolved mass spectrometry for differentiation of the fluorine substitution position on the phenyl ring of fluoromethcathinones.

A reliable method for structural analysis is crucial for the forensic investigation of new psychoactive substances (NPSs). Towards this end, mass spectrometry is one of the most efficient and facile methods for the identification of NPSs. However, the differentiation among 2-, 3-, and 4-fluoromethcathinones (o-, m-, and p-FMCs), which are ring-fluorinated positional isomers part of the major class of NPSs referred to as synthetic cathinones, remains a challenge.

Molecularly imprinted polymer solid-phase extraction of synthetic cathinones from urine and whole blood samples.

In forensic drug analysis, extractive pretreatment is required prior to instrumental analysis to ensure successful detection of the target compounds. However, conventional extraction methods such as hydrophilic polymer-based solid-phase extraction and liquid-liquid extraction are unsuitable for an emerging class of new psychoactive substances, namely, synthetic cathinones, because they exhibit a lack of class selectivity and increased risk of target analyte decomposition during extraction. To address these issues, we describe a highly class-selective sample clean-up method for the extraction of synthetic cathinones from urine and whole blood samples, exploiting a molecularly imprinted polymer solid-phase extraction cartridge.

Differentiation of AB-FUBINACA and its five positional isomers using liquid chromatography-electrospray ionization-linear ion trap mass spectrometry and triple quadrupole mass spectrometry.

Purpose: Positional isomer differentiation is crucial for forensic analysis. The aim of this study was to differentiate AB-FUBINACA positional isomers using liquid chromatography (LC)-electrospray ionization (ESI)-linear ion trap mass spectrometry (LIT-MS) and LC-ESI-triple quadrupole mass spectrometry (QqQ-MS).

Methods: AB-FUBINACA, its two fluorine positional isomers on the phenyl ring, and three methyl positional isomers in the carboxamide side chain were analyzed by LC-ESI-LIT-MS and LC-ESI-QqQ-MS.

Differentiation of AB-FUBINACA positional isomers by the abundance of product ions using electron ionization-triple quadrupole mass spectrometry.

Mass spectrometric differentiation of structural isomers is important for the analysis of forensic samples. Presently, there is no mass spectrometric method for differentiating halogen positional isomers of cannabimimetic compounds. We describe here a novel and practical method for differentiating one of these compounds, N-(1-amino-3-methyl-1-oxobutan-2-yl)-1-(4-fluorobenzyl)-1H-indazole-3-carboxamide (AB-FUBINACA (para)), and its fluoro positional (ortho and meta) isomers in the phenyl ring by electron ionization-triple quadrupole mass spectrometry.

Highly Sensitive Detection of Organophosphorus Pesticides Using 5,10,15,20-Tetrakis(4-hydroxyphenyl)porphyrin.

We describe a unique UV-visible absorption spectral property of 5,10,15,20-tetrakis(4-hydroxyphenyl)porphyrin (THPP) in the presence of organophosphorus (OP) pesticides. Upon titrating each 16 among total 40 different OP pesticides, the Soret band was significantly red-shifted, and a very intense Q band appeared. They were attributed to the diprotonation of THPP.

Characterization of the chemical diversity of glycosylated mycosporine-like amino acids in the terrestrial cyanobacterium Nostoc commune.

Mycosporine-like amino acids (MAAs) are UV-absorbing pigments, and structurally unique glycosylated MAAs are found in the terrestrial cyanobacterium Nostoc commune. In this study, we examined two genotypes of N.commune colonies with different water extract UV-absorption spectra.

Analysis of 11-nor-Δ9 -tetrahydrocannabinol-9-carboxylic acid and its glucuronide in urine by capillary electrophoresis/mass spectrometry.

Δ(9) -Tetrahydrocannabinol is the primary psychoactive component in cannabis, one of the most commonly used illicit drugs in the world. This paper describes a simple and rapid method for direct analysis of major metabolites of Δ(9) -tetrahydrocannabinol; 11-nor-Δ(9) -tetrahydrocannabinol-9-carboxylic acid and its glucuronide in urine by capillary electrophoresis/mass spectrometry. The only pretreatment needed for a urine sample was dilution with methanol containing an internal standard and centrifugation.

Analysis of phosphorus-containing amino acid-type herbicides by sheathless capillary electrophoresis/electrospray ionization-mass spectrometry using a high sensitivity porous sprayer.

We describe a new practical capillary electrophoresis/electrospray ionization-mass spectrometry (CE/ESI-MS) method for the forensic analysis of phosphorus-containing amino acid-type herbicides, glyphosate (GLYP), glufosinate (GLUF) and bialaphos (BIAL). A new sheathless interface, a high sensitivity porous sprayer (HSPS), was used in this study. The limits of detections of GLYP, GLUF and BIAL were 7.