Journal of Analytical Toxicology
October 1, 1996
H. J. Helmlin, K. Bracher, Daniel Bourquin et al.
160 citations
MDMA (Ecstasy) is a widely abused illicit drug at European all-night dance parties. Analytical methods were established to detect MDMA and its metabolites (HMMA, HHMA, MDA, HMA, HHA) in plasma and urine. Plasma and urine samples from two participants in a controlled clinical study were analyzed using high-performance liquid chromatography and gas chromatography-mass spectrometry. After a single oral dose of 1.5 mg/kg MDMA, peak plasma levels of 331 ng/mL MDMA occurred at 2 hours, and 15 ng/mL MDA at 6.3 hours. Peak urine MDMA concentration was 28.1 micrograms/mL at 21.5 hours. Conjugated HMMA and HHMA are the main urinary metabolites.
Journal of Analytical Toxicology
October 1, 1996
J. C. Callaway, Lionel P. Raymon, William Lee Hearn et al.
158 citations
After ritual ingestion of ayahuasca, the highest plasma concentrations in 15 healthy male volunteers were 222.3 ng/mL for harmine, 134.5 ng/mL for tetrahydroharmine, and 9.4 ng/mL for harmaline, with N,N-dimethyltryptamine (DMT) also quantitated. Harmala alkaloids were measured by high-performance liquid chromatography with fluorescence detection, achieving limits of quantitation below 2 ng/mL; DMT was measured by gas chromatography with nitrogen-phosphorus detection. Recovery was quantitative for all analytes. These are the first reported measurements of DMT and harmala alkaloids in human plasma following ritual ayahuasca ingestion. The methods may apply to other biological matrices.
Journal of Analytical Toxicology
January 1, 2005
Jason H Sklerov, Barry Levine, Karla A. Moore et al.
142 citations
A 25-year-old white male died after consuming herbal extracts containing beta-carbolines and hallucinogenic tryptamines. Autopsy found no anatomic cause of death. Toxicologic analysis of heart blood identified N,N-dimethyltryptamine (0.02 mg/L), 5-methoxy-N,N-dimethyltryptamine (1.88 mg/L), tetrahydroharmine (0.38 mg/L), harmaline (0.07 mg/L), and harmine (0.17 mg/L). The medical examiner ruled the cause of death as hallucinogenic amine intoxication and the manner of death as undetermined.
Journal of Analytical Toxicology
March 4, 2015
Nathalie A. Desrosiers, Johannes G. Ramaekers, Émeline Chauchard et al.
136 citations
THC, the main psychoactive compound in cannabis, impairs psychomotor performance, cognition, and driving ability. Occasional cannabis smokers showed significantly more difficulty compensating for tracking error and greater decline in divided attention performance than frequent smokers after smoking one 6.8% THC cigarette. No differences between groups were found on working memory or risk-taking tasks. The results suggest that frequent users develop some tolerance to psychomotor impairment, with implications for driving under the influence cases.
Journal of Analytical Toxicology
April 1, 2002
Nieves Pizarro, Jordi Ortuño, Mercè Farré et al.
113 citations
A gas chromatography-mass spectrometry method simultaneously measured MDMA and its metabolites MDA, HMMA, and HMA in plasma and urine from healthy volunteers given 100 mg of MDMA. Samples were hydrolyzed, extracted with solid-phase columns, and analyzed as trifluoroacyl derivatives. Linear calibration covered plasma and urine ranges of 25–400 ng/mL and 250–2000 ng/mL for MDMA and HMMA, and 2.5–40 ng/mL and 100–1000 ng/mL for MDA and HMA. A capillary electrophoresis method using (2-hydroxy)propyl-beta-cyclodextrin as chiral selector resolved enantiomers without derivatization, with linear ranges for each enantiomer of MDMA, MDA, and HMMA. Stereoselective disposition of MDMA and MDA was confirmed, while HMMA showed an enantiomer ratio near 1 and constant over time, contradicting MDMA findings.
Journal of Analytical Toxicology
January 1, 1998
M J Bogusz, R D Maier, K D Krüger et al.
111 citations
A single, universal solid-phase extraction method using C18 cartridges efficiently extracts a wide range of opiate agonists, cocaine metabolites, and LSD from blood, serum, urine, and other biological fluids. The method achieves high recoveries for most drugs and produces clean extracts suitable for analysis by liquid chromatography coupled with atmospheric-pressure chemical-ionization mass spectrometry. The procedure was developed for routine forensic toxicology casework and demonstrates broad applicability across different drug classes and biological matrices.
Journal of Analytical Toxicology
September 16, 2015
Justin L. Poklis, Stephen A. Raso, Kylie N. Alford et al.
93 citations
NBOMe derivatives, a class of designer hallucinogenic drugs that act as 5-HT2A receptor agonists, have become popular drugs of abuse and can cause severe intoxications, including serotonin-like syndrome with bizarre behavior, severe agitation, and seizures lasting up to 3 days. The most commonly reported derivatives are 25I-NBOMe, 25B-NBOMe, and 25C-NBOMe, often sold on blotter paper. Analysis of three commercial blotter papers using Direct Analysis in Real Time mass spectrometry and high-performance liquid chromatography triple quadrupole mass spectrometry found each contained a different major NBOMe derivative, along with minute amounts of two or three other NBOMe derivative impurities.
Journal of Analytical Toxicology
October 1, 2001
James C. Kraner, Damon Mccoy, Mark A. Evans et al.
89 citations
Recreational use of MDMA (Ecstasy) has risen, especially among young people at raves. Paramethoxyamphetamine (PMA), structurally and pharmacologically similar to MDMA but a more potent central stimulant affecting serotonin, has caused fatalities in Australia and now three in the midwestern United States. The decedents—two males aged 19 and 24 and a female aged 18—believed they were ingesting MDMA but had postmortem blood PMA concentrations of 1.07, 0.60, and 1.90 mg/L, with no MDMA detected. Symptoms included agitation, bruxism, severe hyperthermia, convulsions, and hemorrhage. PMA is metabolized by cytochrome P450 2D6, which is genetically polymorphic; slow metabolizers may have higher peak blood concentrations. The Marquis Test can distinguish PMA from MDMA: MDMA yields dark purple, PMA no color change. PMA pills often bear a Mitsubishi symbol.
Journal of Analytical Toxicology
September 1, 2004
Shawn P Vorce, Jason H Sklerov
79 citations
A gas chromatography-mass spectrometry method was developed to screen for six designer tryptamines and phenethylamines recently added to the DEA's controlled substances list. The method detects pentafluoropropionic derivatives of AMT, DMT, 2CB, DPT, 2C-T-7, and 5-MeO-DiPT, with detection limits of 5-10 ng/mL and linearity from 50 to 1000 ng/mL. It was successfully applied to blood and urine from suspected AMT intoxications. Confirmation of 5-MeO-DiPT in one subject's urine by liquid chromatography-mass spectrometry yielded a concentration of 229 ng/mL, with linearity from 25 to 1500 ng/mL and a detection limit of 5 ng/mL. Two additional peaks suggested metabolites 5-MeO-iPT and 5-MeO-DiPT-N-oxide.
Journal of Analytical Toxicology
March 1, 2000
M Bogusz, Klaus-Dieter Krüger, R. D. Maier
79 citations
A method using liquid chromatography coupled with atmospheric pressure chemical ionization mass spectrometry (LC-APCI-MS) can separate and identify a wide range of phenethylamines, including amphetamine, methamphetamine, and several designer drugs (MDA, MDEA, MDMA, MBDB, BDMPEA), as well as other related compounds like ephedrine and cathinone, from human serum. The drugs are extracted via solid-phase extraction and then analyzed in a single run. The technique provides clear differentiation between all tested drugs, with detection limits between 1 and 5 micrograms per liter of serum and recoveries ranging from 58 to 96%. The method is suitable for routine forensic toxicology analysis of these substances.
Journal of Analytical Toxicology
January 1, 2003
Robert Meatherall, Pankaj Sharma
77 citations
A 21-year-old man ingested a pill called Foxy, containing the hallucinogen 5-methoxy-N,N-diisopropyltryptamine. In the hospital he experienced mild hallucinations and could not move his limbs for about two hours. A urine sample collected four hours after ingestion showed the drug at 1.7 micrograms per milliliter and its metabolite 5-methoxy-indole acetic acid at 1.3 micrograms per milliliter, identified by gas chromatography-mass spectrometry. Two other compounds, tentatively identified as 5-methoxy-N-isopropyltryptamine and 5-methoxy-N,N-diisopropyltryptamine-N'-oxide, were also found. The patient was discharged without follow-up.
Journal of Analytical Toxicology
October 12, 2020
Kelly Francisco da Cunha, Karina Diniz Oliveira, Marilyn A. Huestis et al.
73 citations
A new LC-MS-MS method can detect 104 drugs of abuse, including synthetic cannabinoids, cathinones, fentanyl analogues, and other psychoactive compounds, in oral fluid samples collected with a Quantisal™ device. The method uses a 13.5-minute run and achieves limits of detection as low as 0.05 ng/mL for most analytes, though some require higher concentrations. Matrix effects are generally around 60%, and recoveries range from 47.2% to 127%. Drug stability is best at -20°C, but even frozen, some synthetic cannabinoids degrade more than 20% over 90 days. The method was successfully tested on seven authentic samples, confirming 17 different analytes.
Journal of Analytical Toxicology
January 1, 1996
Jianyi Cai, Jack D. Henion
71 citations
The in vitro metabolism of LSD by human liver microsomes was investigated using tandem mass spectrometry, high-performance liquid chromatography, and capillary electrophoresis. Two new metabolites, lysergic acid ethylamide (LAE) and 2-oxo-LSD, were positively identified by comparison with reference standards. Other detected metabolites included mono- and trioxylated forms. The major metabolic route is deethylation. In human urine specimens from LSD users, iso-LSD was present at the highest concentration, followed by nor-LSD and isonor-LSD, with low levels of LAE and iso-LAE also found.
Journal of Analytical Toxicology
October 1, 1999
Dale K. Hensley, John T. Cody
70 citations
A new method simultaneously measures the ratio of l- and d-enantiomers of amphetamine, methamphetamine, MDA, MDMA, and MDEA in urine. The assay uses liquid-liquid extraction, derivatization with l-TPC, and gas chromatography-mass spectrometry. It provides accurate results for amphetamine and methamphetamine at concentrations of 10 ng/mL or higher and for MDA, MDMA, and MDEA at 25 ng/mL or higher. In eight subjects from a controlled MDMA study, the percentage of l-MDMA was initially greater and increased over time. For the metabolite MDA, the d-enantiomer initially dominated, but the l-enantiomer proportion gradually increased, exceeding the d-enantiomer within 36 hours postdose.
Journal of Analytical Toxicology
October 1, 2003
Byron Curtis, Philip Kemp, Linda Harty et al.
69 citations
2,5-Dimethoxy-4-n-propylthiophenethylamine (2C-T-7), a compound similar to MDMA, was identified in a routine postmortem screening of a 20-year-old man who died after reportedly insufflating 35 mg. A quantitative method for detecting 2C-T-7 in blood, urine, and liver was developed using liquid-liquid extraction and gas chromatography with nitrogen-phosphorus detection and mass spectrometry. Detection and quantitation limits in blood were 6.0 and 15.6 ng/mL. In the case, heart blood contained 57 ng/mL, femoral blood 100 ng/mL, urine 1120 ng/mL, and liver 854 ng/g.
Journal of Analytical Toxicology
April 20, 2022
Amanda L A Mohr, Barry K. Logan, Melissa F. Fogarty et al.
66 citations
A critical review of published case reports from January 2017 through December 2020 identified 1,319 cases of adverse events associated with novel psychoactive substances (NPS), including 378 overdose fatalities, 771 cases requiring clinical treatment or hospitalization, and 170 cases of driving under the influence. The review covers chemistry, pharmacology, user profiles, and clinical symptoms for over 60 NPS, with 50 substances reported for the first time compared to the previous four years. Cases span synthetic cannabinoids, NPS stimulants, hallucinogens, benzodiazepines, and opioids. The findings aim to improve awareness and characterization of emerging international drug threats.
Journal of Analytical Toxicology
July 1, 2003
Simona Pichini, M.d. Sánchez Navarro, Roberta Pacifici et al.
66 citations
After a single 100-mg dose of MDMA, the drug appears in sweat within 1.5 hours and peaks at 24 hours, but the amount varies up to 30-fold between individuals, ranging from 3.2 to 1326.1 ng per patch. Only traces of the metabolite MDA are detected. An onsite sweat strip test is positive at 1.5 hours, though 18% false-negative results occur in the first 6 hours. Sweat patch and onsite strip testing offer noninvasive ways to monitor MDMA use.
Journal of Analytical Toxicology
November 1, 2003
Frank T. Peters, Nele Samyn, Martin Wahl et al.
65 citations
The pharmacological effects of amphetamine, methamphetamine, MDA, MDMA, and MDEA depend on their mirror-image molecular forms (enantiomers), which differ in how they act in the body. Analysis of plasma from clinical toxicology cases and from drivers suspected of drug impairment showed that concentrations of most enantiomers were lower in routine screening samples than in intoxication or driving-under-the-influence cases. Drivers under the influence had higher levels of both amphetamine enantiomers than intoxicated patients. Differences in the ratio of R to S enantiomers for several drugs between groups suggest these ratios can help distinguish recent from past use. In one MDMA poisoning, the R form cleared more slowly (half-life 6.0 hours) than the S form (4.1 hours), and the ratio of R to S rose over time.
Journal of Analytical Toxicology
July 1, 2005
Diane M. Boland, Wilmo Andollo, George W. Hime et al.
62 citations
Alpha-methyltryptamine (AMT), an indole analogue of amphetamine originally investigated as an antidepressant and monoamine oxidase inhibitor, caused the first known death in the United States when a young college student in Miami-Dade County died after ingesting the drug. The student told his roommate he was taking hallucinating drugs and had discovered the secret of the universe; about 12 hours later he was found unresponsive in bed with an empty 1-gram vial of AMT. Postmortem blood showed 2.0 mg/L of AMT, the liver contained 24.7 mg/kg, and the brain contained 7.8 mg/kg. AMT was emergency-scheduled as a Schedule 1 controlled substance shortly after this death.
Journal of Analytical Toxicology
March 1, 2002
Tatsuyuki Kanamori, Hiroyuki Inoue, Yuko T Iwata et al.
61 citations
In rats, the psychoactive compound 2C-B is broken down into at least six distinct breakdown products through two main metabolic pathways. One pathway converts 2C-B into an aldehyde, which is then further processed into an alcohol and a carboxylic acid. The other pathway produces metabolites where a methyl group is removed from either the 2- or 5-position of the molecule, followed by acetylation of the amino group. These findings indicate that the body metabolizes 2C-B through multiple chemical changes, resulting in a variety of metabolites that are excreted in urine.
Journal of Analytical Toxicology
January 1, 1998
Olof Beck, Anders Helander, Christine Karlson-Stiber et al.
58 citations
Mushrooms containing psilocybin are often used for intentional intoxication, sometimes leading to adverse reactions with tachycardia that psilocybin alone does not explain. This study detected phenylethylamine in Psilocybe semilanceata using gas chromatography-mass spectrometry and found its amount varies more than psilocybin. The highest phenylethylamine level, 146 micrograms per gram wet weight, came from mushrooms involved in a case where three young men were hospitalized. Comparing symptoms from magic mushroom intoxication with those from pure psilocybin or phenylethylamine suggests phenylethylamine may contribute to adverse reactions.
Journal of Analytical Toxicology
September 1, 1998
C Giroud, M Augsburger, L Rivier et al.
57 citations
Two sets of tablets from the Swiss black market were analyzed to identify 4-bromo-2,5-dimethoxyphenethylamine (2C-B) using multiple analytical methods including GC-MS, HPLC-DAD, CE-DAD, FTIR, and NMR. Only a combination of mass spectrometry and NMR provided unequivocal identification. Quantitation by HPLC-DAD and CE-DAD showed the tablets contained 3 to 8 mg of 2C-B, which is within the minimum amount needed to produce the drug's characteristic effects.
Journal of Analytical Toxicology
October 1, 2009
T. T. Abraham, Allan J. Barnes, Richie H. Lowe et al.
56 citations
After a single oral dose of MDMA (ecstasy), the drug and its metabolites are excreted in urine over an extended period, with the metabolite HMMA detectable longer than MDMA itself. In a double-blind study, healthy adult MDMA users received placebo, 1.0 mg/kg, or 1.6 mg/kg doses. From 916 urine specimens provided by 16 participants, median peak concentrations after the higher dose were 21,470 ng/mL for MDMA and 20,793 ng/mL for HMMA, with HMMA's last detection exceeding MDMA's by over 33 hours. In the first 24 hours, 30.2-34.3% of total urinary excretion occurred. Including HMMA in urine testing improves detection of MDMA exposure but requires hydrolysis of the sample.
Journal of Analytical Toxicology
January 1, 1988
Paula Francom, David M. Andrenyak, Hyun Kyoon Lim et al.
55 citations
A method detects LSD in urine at concentrations as low as 0.5 ng/mL. After adding a deuterium-labeled internal standard, LSD is extracted from urine at pH 8 using n-butyl chloride, then converted to a trimethylsilyl derivative and measured by gas chromatography–mass spectrometry with selected ion monitoring. The procedure tracked LSD concentrations in urine for eight hours after two volunteers each took 70.5 micrograms of LSD orally. Results are compared with those from radioimmunoassay and high-performance liquid chromatography. The report also includes data on LSD stability in urine.
Journal of Analytical Toxicology
February 19, 2015
Simon Elliott, Simon D. Brandt, Jason Wallach et al.
54 citations
2-Methoxydiphenidine (2-MXP), a dissociative research chemical sold as an alternative to methoxetamine and ketamine, was detected in post-mortem blood and urine from three fatalities. Femoral blood concentrations were 24.0, 2.0, and 1.36 mg/L; the lowest case had an alternative cause of death. Therapeutic levels of prescription drugs were also present. Metabolites included hydroxy-2-MXP (with hydroxylation on the piperidine ring), O-desmethyl-2-MXP, and hydroxylated O-desmethyl-2-MXP. Diphenidine and hydroxy-diphenidine were detected, but it was unclear if they came from 2-MXP or separate diphenidine use. These are the first published fatalities involving 2-MXP, providing analytical data for forensic toxicologists.