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Analytical Chemistry

ISSN 0003-2700

4 papers in the library · 273 citations · publishing 1988-2019

Papers

On-Line Immunoaffinity Extraction-Coupled Column Capillary Liquid Chromatography/Tandem Mass Spectrometry: Trace Analysis of LSD Analogs and Metabolites in Human Urine

Analytical Chemistry January 1, 1996 Jianyi Cai, Jack D. Henion 112 citations

An on-line immunoaffinity extraction-coupled column capillary liquid chromatography/tandem mass spectrometry method was developed to detect LSD and its analogs and metabolites in human urine. The system uses three columns and allows direct analysis of diluted urine without pretreatment, eliminating sample handling steps. Concentrations as low as 2.5 parts per trillion of LSD and several analogs were detected in spiked human urine, which is 20-fold lower than the previous limit of detection using solid phase extraction and liquid chromatography/tandem mass spectrometry. The method was also applied to urine specimens from LSD users.

Quantification of LSD and N-demethyl-LSD in urine by gas chromatography/resonance electron capture ionization mass spectrometry

Analytical Chemistry July 15, 1988 Hyun Kyoon Lim, David M. Andrenyak, Paula Francom et al. 68 citations

A gas chromatography/resonance electron capture ionization mass spectrometry method was developed to quantify LSD and its metabolite N-demethyl-LSD in urine. The method achieved detection limits of 0.1 ng/mL for LSD and 0.2 ng/mL for N-demethyl-LSD, with linear calibration curves over a range of 0.5 to 20 ng/mL. The technique was applied to urine samples from human subjects administered known doses of LSD, demonstrating reliable identification and measurement of both compounds. The approach offers improved sensitivity and specificity for forensic and clinical detection of LSD use.

Determination of lysergic acid diethylamide (LSD), iso-LSD, and N-demethyl-LSD in body fluids by gas chromatography/tandem mass spectrometry

Analytical Chemistry July 15, 1992 Chad C. Nelson, Rodger L. Foltz 64 citations

Capillary gas chromatography/tandem mass spectrometry (GC/MS/MS) methods can detect and quantify LSD, iso-LSD, and N-demethyl-LSD in urine or blood at low-pg/mL concentrations. Derivatization, sample introduction, and ionization techniques were evaluated for efficiency and specificity. Fragmentation pathways from collision-induced dissociation show principal losses from the amide and piperidine-ring moieties. Positive-ion ammonia chemical ionization with MS/MS analysis of trimethylsilyl derivatives provides high specificity for identifying these compounds. Negative-ion chemical ionization with GC/MS/MS of the trifluoroacetyl derivative is suited for trace-level identification of N-demethyl-LSD, a metabolite.

Setup of a Serotonin 2A Receptor (5-HT2AR) Bioassay: Demonstration of Its Applicability To Functionally Characterize Hallucinogenic New Psychoactive Substances and an Explanation Why 5-HT2AR Bioassays Are Not Suited for Universal Activity-Based Screening of Biofluids for New Psychoactive Substances

Analytical Chemistry November 14, 2019 Eline Pottie, Annelies Cannaert, Katleen van Uytfanghe et al. 29 citations

Classic hallucinogens, which activate the serotonin 2A receptor (5-HT2AR), represent the third largest category of new psychoactive substances. A new bioassay was developed that measures receptor activation by monitoring β-arrestin2 recruitment using a split-luciferase system. The assay determined potency and efficacy for various hallucinogens, including LSD, 5-MeO-DALT, mescaline, and several 2C compounds and their NBOMe derivatives, with EC50 values ranging from subnanomolar (NBOMes) to micromolar (mescaline) levels. When applied to plasma screening, blank samples showed pronounced receptor activation due to endogenous serotonin, confirmed by its elimination with a 5-HT2AR antagonist or MAO-A treatment, and by LC-HRMS analysis. The bioassay's main application is characterizing poorly understood serotonergic hallucinogens, as MAO-A metabolism of some compounds could bias detection in biofluids.