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Analytical and bioanalytical chemistry

ISSN 1618-2650

10 papers in the library · 298 citations · publishing 2010-2025

Papers

LC-MS/MS screening method for designer amphetamines, tryptamines, and piperazines in serum.

Analytical and bioanalytical chemistry April 1, 2010 Ariane Wohlfarth, Wolfgang Weinmann, Sebastian Dresen 128 citations

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method can simultaneously identify 35 substances, including 31 new designer drugs plus cathinone, methcathinone, phencyclidine, and ketamine. The method covers amphetamine derivatives (e.g., 2C-B, DOB, PMA), tryptamine derivatives (e.g., DMT, 5MeO-DMT), and piperazine derivatives (e.g., BZP, mCPP). After solid-phase extraction and gradient elution, detection limits range from 1.0 to 5.0 ng/mL, matrix effects from 65% to 118%, and extraction efficiencies from 72% to 90%. The assay is selective for all tested substances.

Metabolism of the new psychoactive substances N,N-diallyltryptamine (DALT) and 5-methoxy-DALT and their detectability in urine by GC-MS, LC-MSn, and LC-HR-MS-MS.

Analytical and bioanalytical chemistry October 1, 2015 Julian A Michely, Andreas G Helfer, Simon D Brandt et al. 49 citations

N,N-Diallyltryptamine (DALT) and 5-methoxy-DALT (5-MeO-DALT) are synthetic tryptamines with psychoactive effects. In rats, after high-dose administration, their metabolism involves aromatic and aliphatic hydroxylations, N-dealkylation, N-oxidation, and combinations; 5-MeO-DALT also undergoes O-demethylation, followed by extensive glucuronidation or sulfation. The main cytochrome P450 enzymes for DALT are CYP2C19, CYP2D6, and CYP3A4; for 5-MeO-DALT, CYP1A2, CYP2C19, CYP2D6, and CYP3A4. For detecting low-dose consumption in rat urine, LC-MS(n) and LC-HR-MS-MS are suitable; the most abundant markers are a ring hydroxy metabolite of DALT, the N,O-bis-dealkyl metabolite of 5-MeO-DALT, and their glucuronides. GC-MS can screen DALT only via its main metabolites.

A qualitative/quantitative approach for the detection of 37 tryptamine-derived designer drugs, 5 β-carbolines, ibogaine, and yohimbine in human urine and plasma using standard urine screening and multi-analyte approaches.

Analytical and bioanalytical chemistry January 1, 2014 Markus R Meyer, Achim Caspar, Simon D Brandt et al. 39 citations

A new laboratory method using liquid chromatography and linear ion trap mass spectrometry can detect 37 synthetic tryptamines plus five β-carbolines, ibogaine, and yohimbine in human urine and plasma. The method is selective for all tested substances, with detection limits in urine between 10 and 100 ng/mL and in plasma between 1 and 100 ng/mL. Validated quantification in plasma was achieved for 33 of the 44 analytes. This addresses the previous scarcity of analytical data on detecting these emerging designer drugs in human biosamples.

Biotransformation and detectability of the new psychoactive substances N,N-diallyltryptamine (DALT) derivatives 5-fluoro-DALT, 7-methyl-DALT, and 5,6-methylenedioxy-DALT in urine using GC-MS, LC-MSn, and LC-HR-MS/MS.

Analytical and bioanalytical chemistry February 1, 2017 Julian A Michely, Simon D Brandt, Markus R Meyer et al. 23 citations

Derivatives of N,N-diallyltryptamine (DALT) are new psychoactive substances. Their metabolism and detectability were studied in rat urine and human liver microsomes using liquid chromatography-high resolution-tandem mass spectrometry. Main metabolic pathways include aromatic and aliphatic hydroxylations, N-dealkylation, N-oxidation, and combinations; carboxylation was detected for 7-Me-DALT and O-demethylenation for 5,6-MD-DALT. Phase I metabolites were extensively glucuronidated or sulfated, catalyzed by several CYP isoenzymes. GC-MS could not reliably monitor consumption, but LC-MSn and LC-HR-MS/MS approaches were suitable, especially for detecting 5-F-DALT and 7-Me-DALT at low doses. The most abundant targets for each compound are specified.

Forensic analysis of Salvia divinorum using multivariate statistical procedures. Part I: discrimination from related Salvia species.

Analytical and bioanalytical chemistry January 1, 2012 Melissa A Bodnar Willard, Victoria L Mcguffin, Ruth Waddell Smith 15 citations

Salvinorin A, the active compound in the hallucinogenic herb Salvia divinorum, was extracted from its leaves in five minutes using dichloromethane. Four other Salvia species (Salvia officinalis, Salvia guaranitica, Salvia splendens, and Salvia nemorosa) were extracted the same way, and all extracts were analyzed by gas chromatography-mass spectrometry. Visual inspection of the chromatograms distinguished S. divinorum from the others. For a more objective comparison, the total ion chromatograms were processed with principal components analysis after data pretreatment to reduce non-chemical variance. The resulting scores plot also allowed visual discrimination. Numerical assessments using Euclidean distance, hierarchical cluster analysis, t tests, Wilcoxon rank-sum tests, and Pearson correlation were applied to the PCA scores, and these statistical procedures were compared for their forensic usefulness.

Determination of synthetic hallucinogens in oral fluids by microextraction by packed sorbent and liquid chromatography-tandem mass spectrometry.

Analytical and bioanalytical chemistry July 1, 2023 Evan Lesne, Miguel Muñoz-Bartual, Francesc A Esteve-Turrillas 14 citations

A fast and simple method using microextraction by packed sorbent and liquid chromatography-tandem mass spectrometry was developed to simultaneously quantify 28 synthetic hallucinogens in oral fluids, including LSD and substances from NBOMe, NBOH, NBF, 2C, and substituted amphetamine classes. Optimal extraction used C18 sorbent, 100 μL sample at pH 7 loaded in 3 cycles, washing with water, and eluting with 50 μL methanol in 1 cycle, yielding quantitative recoveries (80–129%) and no significant matrix effects. Limits of detection ranged from 0.09 to 1.22 μg L⁻¹. Precision was high, with relative standard deviations below 9%. The method is appropriate for simple, sensitive determination of NBOMe derivatives and other synthetic hallucinogens in oral fluid samples.

Biotransformation and detectability of the designer drug 2,5-dimethoxy-4-propylphenethylamine (2C-P) studied in urine by GC-MS, LC-MS(n), and LC-high-resolution-MS(n).

Analytical and bioanalytical chemistry January 1, 2015 Carina S D Wink, Markus R Meyer, Tina Braun et al. 13 citations

2C-P is a hallucinogenic designer drug from the phenethylamine class. This work identified its phase I and II metabolites and tested detectability in urine. Proposed metabolic pathways include N-acetylation, deamination with reduction to alcohol or oxidation to carbonic acid, mono- and bis-hydroxylation, mono- and bis-O-demethylation followed by glucuronidation or sulfation, and combinations. A common user's dose of 2C-P was reliably detectable in urine using standard GC-MS and LC-MS(n) screening methods, supporting its identification in clinical and forensic cases.

Understanding ayahuasca effects in major depressive disorder treatment through in vitro metabolomics and bioinformatics.

Analytical and bioanalytical chemistry July 1, 2023 Flávia S Zandonadi, Alex Ap Rosini Silva, Aline A S Melo et al. 9 citations

Metabolomic studies of major depressive disorder have focused on energy, oxidative stress, and neurotransmission pathways. Hub metabolites—key nodes in biochemical networks—integrate metabolism and signaling. This work used an in vitro primary astrocyte model with untargeted metabolomics of secretome and intracellular content after ayahuasca treatments based on DMT concentration. Mass spectrometry data identified significant hub metabolites predicting pathway alterations. Ayahuasca treatment was associated with branched-chain amino acid, vitamin B6, and vitamin B3 metabolism as housekeeping pathways. At the lowest DMT concentration (1 µmol L-1), dopamine synthesis was overrepresented in network results. Building reaction networks with metabolites like nicotinamide, L-DOPA, and L-leucine can guide dose decisions and pathway selection in future studies.

Forensic analysis of Salvia divinorum using multivariate statistical procedures. Part II: association of adulterated samples to S. divinorum.

Analytical and bioanalytical chemistry January 1, 2012 Melissa A Bodnar Willard, Victoria L Mcguffin, Ruth Waddell Smith 5 citations

Salvia divinorum, a plant with hallucinogenic properties due to its active ingredient salvinorin A, was studied to see if it could be identified when mixed with other plant materials. The plant was extracted and added to samples of S. divinorum, Salvia officinalis, Cannabis sativa, and Nicotiana tabacum to mimic adulterated forensic samples. After extraction and gas chromatography-mass spectrometry analysis, the data were preprocessed and examined with principal components analysis (PCA). Visual inspection of PCA scores plots allowed association of adulterated extracts with unadulterated S. divinorum. Additional statistical tests—Euclidean distance, hierarchical cluster analysis, t tests, Wilcoxon rank-sum tests, and Pearson correlation—provided further evaluation, with their forensic advantages and limitations compared.

A novel method for the determination of synthetic cathinones and related substances in postmortem blood samples using cork-based dispersive solid-phase microextraction prior to LC-MS/MS analysis.

Analytical and bioanalytical chemistry May 14, 2025 Letícia Birk, Bruno Pereira Dos Santos, Sarah Eller et al. 3 citations

A new method using cork powder as a biosorbent in solid-phase microextraction combined with LC-MS/MS was developed to detect synthetic cathinones and related substances in postmortem blood. The method requires only 200 µL of sample and 30 mg of cork, with a 7.5-minute run time. Validation following ASB/ANSI Standard 036 showed lower limits of quantification between 0.5 and 1 ng/mL and linear ranges up to 85 ng/mL. Accuracy and precision were satisfactory, though significant ion suppression (2.9-63.4%) was observed. Testing on three forensic postmortem blood samples confirmed MDMA (79.2-198.1 ng/mL) and MDA (23.1-26.6 ng/mL). The method scored 0.53 on the AGREEprep greenness scale, offering a reliable and more environmentally friendly alternative for forensic toxicology.