Journal of Analytical Toxicology
September 1, 1996
Yoshiro Nakahara, Ruri Kikura, Kazunori Takahashi et al.
36 citations
Lysergic acid diethylamide (LSD) and its metabolite norLSD can be detected in hair after administration. In pigmented rats given daily doses of 0.05 to 2 mg/kg for 10 days, LSD was found in newly grown hair even at the lowest dose, while norLSD appeared only at the highest dose. Analysis of hair from 17 self-reported LSD users detected LSD in two samples. The methods used gas chromatography-mass spectrometry and high-performance liquid chromatography with fluorometric detection, demonstrating the feasibility of hair analysis for LSD exposure.
Journal of Analytical Toxicology
April 1, 2011
H. H. Lee, J. F. Lee, Shin‐yu Lin et al.
35 citations
A single analytical protocol using solid-phase extraction, derivatization with heptafluorobutyric anhydride, and gas chromatography-mass spectrometry can simultaneously measure amphetamine, methamphetamine, MDA, MDMA, MDEA, ketamine, and norketamine in urine. With a 1-mL sample, detection limits range from 15 to 70 ng/mL, and upper limits reach 6000–8000 ng/mL. Precision and accuracy are high, with within-day and between-day coefficients of variation ≤4.95% and accuracy between 96.0% and 110.7% for most analytes. Testing on 107 previously positive urine samples showed good agreement with earlier methods, enabling a single confirmation test for samples screening positive for amphetamines, ketamine, or both.
Journal of Analytical Toxicology
July 1, 2016
John J Kristofic, Jeffrey D Chmiel, George F Jackson et al.
34 citations
A 23-year-old Caucasian male died after being subdued by military law enforcement, having experienced severe respiratory distress. Autopsy revealed mild to moderate coronary atherosclerosis, biventricular dilation, mild right ventricular hypertrophy, and bilateral pulmonary edema and congestion. Blood contained no drugs or ethanol, but urine had pseudoephedrine, nicotine, and cotinine. A designer drug screen detected 25C-NBOMe, 25C-NBOH, and 2C-C in blood and urine. 25C-NBOMe concentrations were measured in blood (2.07 ng/mL), urine (27.43 ng/mL), and various organs. The medical examiner ruled the cause of death as 25C-NBOMe toxicity temporally associated with excited delirium and forcible restraint, manner accidental.
Journal of Analytical Toxicology
May 1, 1990
Gary W. Kunsman, Joseph E. Manno, K.r. Cockerham et al.
34 citations
MDMA and MDEA, hallucinogenic amphetamine analogs, are increasingly used recreationally, prompting evaluation of common urine drug tests. The Abbott TDx and Syva EMIT-d.a.u. amphetamine immunoassays were tested for cross-reactivity with MDMA- and MDEA-spiked urine samples. The Syva EMIT assay detected only the highest concentration (10.0 micrograms/mL) of both substances. The TDx assay showed cross-reactivity for MDMA ranging from 18% at high concentrations to 118% at low concentrations, and for MDEA from 12% to 47%. Precision for TDx was good, with coefficients of variation below 6% for MDMA. Negative EMIT but positive TDx results were confirmed by GC/MS.
Journal of Analytical Toxicology
January 1, 2004
K. M. Jenkins, Michael S. Young, Claude R. Mallet et al.
33 citations
A solid-phase extraction method using a mixed-mode cation exchange cartridge effectively cleans and concentrates MDMA and its metabolites MDA and HMMA from urine for analysis by liquid chromatography–mass spectrometry. Recoveries ranged from 88% to 108% across concentrations of 0.10 to 20 micrograms per milliliter. The LC-MS method required the least sample handling, offered the highest throughput, and provided better selectivity for HMMA in real samples compared with LC-UV. GC with nitrogen-phosphorus detection gave comparable selectivity but involved more manipulation, leading to lower recovery and precision. Lower quantitation limits were 0.1 microgram per milliliter for MDMA and MDA and 0.04 microgram per milliliter for HMMA.
Journal of Analytical Toxicology
April 1, 2000
Gregory K. Poch, K. L. Klette, Carolyn J. Anderson
33 citations
Two liquid chromatography methods (mass spectrometry and ion trap mass spectrometry) are compared for detecting 2-oxo-3-hydroxy lysergic acid diethylamide (O-H-LSD), a major LSD metabolite in urine. Both procedures show linear calibration from 0 to 8,000 pg/mL with correlation coefficients above 0.99, and limits of detection and quantitation of 400 pg/mL. Reanalysis of 68 human urine specimens previously positive for LSD found O-H-LSD concentrations averaging about 16 times higher than LSD concentrations. Either method can be adapted for high-volume drug testing, and targeting this metabolite may extend the detection window for LSD use.
Journal of Analytical Toxicology
September 1, 2011
Sarah Kerrigan, Monica Brady Mellon, Stephanie Banuelos et al.
32 citations
Nine commercial enzyme-linked immunosorbent assays (ELISAs) used for routine drug screening fail to detect most psychedelic phenethylamines of the 2C, 2C-T, and DO series. Cross-reactivity for 10 of 11 tested designer drugs was below 0.4%, and even concentrations up to 50,000 ng/mL in urine—far above typical forensic levels—did not trigger a positive result. Only 4-methylthioamphetamine (4-MTA) showed measurable cross-reactivity, ranging from 5% to 200% depending on the assay. Laboratories relying solely on immunoassay screening may therefore miss these powerful psychedelic substances, whereas broad-spectrum chromatographic techniques can detect them.
Journal of Analytical Toxicology
August 10, 2015
Iain M. Mcintyre, Amber Trochta, Ray D. Gary et al.
30 citations
A man with a history of strange behavior was found dead in his locked room. Toxicology testing detected the hallucinogen 4-methoxyphencyclidine (4-MeO-PCP) at a peripheral blood concentration of 8.2 mg/L and a central blood concentration of 14 mg/L. The liver contained 120 mg/kg, vitreous fluid 5.1 mg/L, urine 140 mg/L, and gastric contents 280 mg. Another hallucinogen, 4-hydroxy-N-methyl-N-ethyltryptamine, was also present but not quantified. Therapeutic levels of venlafaxine, olanzapine, lorazepam, and hydroxyzine were confirmed, but phencyclidine was not detected. The death was certified as an accident due to acute mixed drug intoxication.
Journal of Analytical Toxicology
April 3, 2013
Giorgia de Paoli, Simon D. Brandt, Jason Wallach et al.
30 citations
Three psychoactive arylcyclohexylamines sold online as research chemicals were chemically identified: methoxetamine, N-ethyl-1-(3-methoxyphenyl)cyclohexanamine, and 1-[1-(3-methoxyphenyl)cyclohexyl]piperidine. A validated liquid chromatography method with ultraviolet detection reliably measured these compounds in blood, urine, and vitreous humor at concentrations from 0.16 to 5.0 mg/L, while mass spectrometry served as a confirmatory technique.
Journal of Analytical Toxicology
October 1, 2000
J. H. Sklerov, Joseph Magluilo, K. K. Shannon et al.
30 citations
A method measures LSD and its metabolite O-H-LSD in urine and blood. O-H-LSD appears in urine at concentrations many times higher than LSD, extending detection time for confirming LSD use. A single-step liquid-liquid extraction on 5-mL urine samples precedes liquid chromatography with electrospray ionization mass spectrometry. Detection limits are 400 pg/mL for O-H-LSD and 100 pg/mL for LSD. In nine LSD-positive urine samples, mean O-H-LSD concentration was 6378 pg/mL (range 332-21371 pg/mL) and mean LSD concentration was 844 pg/mL (range 177-2456 pg/mL), with O-H-LSD levels 0.9 to 19.8 times higher than LSD (mean 10.2). No O-H-LSD was detected in blood samples. Enzymatic hydrolysis of six urine samples showed no significant difference, indicating absence of glucuronic acid conjugation.
Journal of Analytical Toxicology
October 1, 2017
Michelle Williams, Jennifer Martin, Peter Galettis
29 citations
A validated method detects 32 synthetic stimulant and hallucinogenic drugs, often sold as bath salts, in oral fluid. Using simple protein precipitation and a 7.5-minute chromatographic separation, the technique achieves detection limits of 1 ng/mL and quantitation from 2.5 to 500 ng/mL with high accuracy (85.3-108.4%) and precision (1.9-14%). Applied to 12 routine samples, two contained 2-CB and DOB (5 and 4 ng/mL) and MPBP and TFMPP (both 4 ng/mL). The method enables rapid screening of these compounds in oral fluid, applicable to routine testing laboratories.
Journal of Analytical Toxicology
February 18, 2013
Thomas Berg, Benedicte Jørgenrud, Dag Helge Strand
27 citations
A sensitive analytical method using ultra-performance liquid chromatography-tandem mass spectrometry was developed and validated to measure buprenorphine, fentanyl, and lysergic acid diethylamide (LSD) in whole blood. Sample preparation involved liquid-liquid extraction with methyl tert-butyl ether. The method achieved detection limits of 0.28 ng/mL for buprenorphine, 0.044 ng/mL for fentanyl, and 0.0097 ng/mL for LSD. Most phospholipids were removed during extraction, and matrix effects were minimal or absent. Since September 2011, the method has been routinely used at the Norwegian Institute of Public Health for qualitative and quantitative analysis of over 400 whole blood samples, each tested in duplicate.
Journal of Analytical Toxicology
October 1, 1996
R Kronstrand
27 citations
The psychoactive substance MBDB, a selective serotonin-releasing agent similar to MDMA (ecstasy), was identified in urine samples from ten people suspected of petty drug offenses in Sweden. MBDB concentrations ranged from 0.1 to 24 micrograms per milliliter. Its metabolite BDB was also detected. In seven of the ten samples, MBDB and BDB were the only ecstasy-type compounds present, though other drugs were found. This appears to be the first report of MBDB abuse in Sweden.
Journal of Analytical Toxicology
September 1, 2003
J.l. Henry, Jean A Epley, Timothy P. Rohrig
25 citations
In a death from multiple gunshot wounds, mescaline concentrations were measured in body fluids and tissues: 2.95 mg/L in blood, 2.36 mg/L in vitreous humor, 8.2 mg/kg in liver, and 2.2 mg/kg in brain. The drug was extracted using a butyl chloride liquid-liquid method, identified by mass spectrometry, and quantified by gas chromatography with a nitrogen-phosphorus detector. This report documents the distribution of mescaline in a forensic case, providing data on its postmortem levels in different biological matrices.
Journal of Analytical Toxicology
September 1, 1998
J. Röhrich, Siegfried Zörntlein, Johannes Lotz et al.
25 citations
A routine drug screening using the CEDIA DAU assay falsely identified lysergic acid diethylamide (LSD) in urine samples from 12 intensive care unit patients. None of these positive results were confirmed by high-performance liquid chromatography, but all samples contained the mucolytic drug ambroxol. Further investigation showed that ambroxol significantly cross-reacts with the CEDIA DAU LSD assay. Positive LSD results from this assay require careful evaluation, especially during cold season when mucolytic medications are more commonly used.
Journal of Analytical Toxicology
January 1, 2008
Pamela C Mcdonough, Justin M Holler, Shawn P Vorce et al.
24 citations
A new analytical method using solid-phase extraction with liquid chromatography-electrospray ionization mass spectrometry accurately detects and quantifies the psychoactive compound salvinorin A in human blood and urine. The method reliably measures concentrations between 5.0 and 100 ng/mL, with a detection limit of 2.5 ng/mL and a quantitation limit of 5.0 ng/mL. It provides a robust tool for forensic toxicology to identify salvinorin A in biological fluids, addressing the lack of published methods and supporting research on the compound's health effects and pharmacokinetics.
Journal of Analytical Toxicology
October 1, 2006
R. H. Liu, H.-c. Liu, Dongliang Lin
23 citations
Forensic toxicologists established protocols to detect MDMA (ecstasy) and its metabolite MDA in hair, urine, and postmortem specimens using gas chromatography-mass spectrometry. In 20 fatal cases, MDMA and MDA were measured in heart blood, gastric content, urine, and bile. Additional data came from 25 antemortem urine and 6 hair specimens. The MDA/MDMA ratio in hair was consistent and appeared higher than in other specimens, but the MDMA/MDA ratio in hair did not differ significantly from ratios in urine or blood, similar to patterns seen with cocaine/benzoylecgonine and THC/THC-acid.
Journal of Analytical Toxicology
October 1, 2006
Stéphane Pirnay, T. T. Abraham, Richie H. Lowe et al.
23 citations
Acid hydrolysis recovers more MDMA urinary metabolites than enzymatic hydrolysis with beta-glucuronidase from either E. coli or Helix pomatia. Acid hydrolysis yielded 40.0% and 39.3% higher HMA recovery compared to E. coli and H. pomatia hydrolysis, respectively. E. coli beta-glucuronidase gave 17.1% and 26.5% greater MDA recovery than acid hydrolysis and H. pomatia hydrolysis. HMMA recovery by acid hydrolysis was 336.1% and 159.8% greater than E. coli and H. pomatia beta-glucuronidase. Optimal conditions were 100 µL hydrochloric acid per 1 mL urine incubated at 120°C for 40 minutes. Based on recovery, time, availability, and cost, acid hydrolysis is preferred.
Journal of Analytical Toxicology
October 1, 1997
S. J. Salamone, Z. Li, A. J. Mcnally et al.
23 citations
LSD converts to its epimer iso-LSD at temperatures above 37 °C and pH levels over 7.0. At pH 7.0 or higher, a 9:1 ratio of LSD to iso-LSD is reached after one week at 45 °C or two weeks at 37 °C. Starting from iso-LSD, achieving the same 9:1 ratio requires six weeks at 45 °C and pH 9.7, indicating more vigorous conditions are needed. This ratio represents an equilibrium concentration with an equilibrium constant K = 9. The study used proton NMR to follow the reaction by integrating the C-9 resonances of LSD and iso-LSD, appearing as singlets at 6.35 and 6.27 ppm respectively. This is the first quantitative measurement of LSD epimerization by NMR.
Journal of Analytical Toxicology
July 11, 2016
Maria Nieddu, Lucia Burrai, Elena Baralla et al.
22 citations
Thirty new amphetamine designer drugs were tested for cross-reactivity with two commercial immunoassay kits (Neogen® Amphetamine Specific and Methamphetamine/MDMA assays) in whole blood, urine, and oral fluid. For most of the designer drugs, concentrations as high as 10,000 ng/mL failed to produce a positive response. This shows that while the kits work well for their target drugs—amphetamine, methamphetamine, and MDMA—they cannot reliably detect the tested designer drugs in real forensic cases because the required concentrations far exceed those typically found in biological samples.
Journal of Analytical Toxicology
July 1, 2003
Peter Stout, K. L. Klette, Russell Wiegand
21 citations
Four immunoassays for detecting amphetamine, methamphetamine, MDA, and MDMA were tested on about 27,500 human urine samples and 7,000 control samples over eight days. The DRI ecstasy reagent detected about 23% more MDMA-positive samples than the ONLINE reagent and had a confirmation rate near 90%. The modified ONLINE reagent, which included sodium periodate and was calibrated with MDMA, performed poorly, with control failure rates up to 38.3% and no improved MDMA sensitivity. The DRI methamphetamine reagent had a low confirmation rate (6% or less) and frequently gave positive results for samples containing only ephedrine or pseudoephedrine.
Journal of Analytical Toxicology
January 29, 2020
Xiuying Yan, Ping Xiang, Yunli Zhao et al.
20 citations
A method using gas chromatography high-resolution mass spectrometry was developed to detect and measure the designer hallucinogen 5-MeO-DIPT in urine. Two metabolites, 5-OH-DIPT and 5-MeO-IPT, were identified in users' urine. The method accurately quantified 5-MeO-DIPT between 2 and 300 ng/mL, with a detection limit of 1 ng/mL. In drug abusers, urine concentrations ranged from 1 to 2.8 ng/mL. Stability testing showed that 5-MeO-DIPT concentration decreased by 22.8% after 24 hours at 25°C, 33.2% after 5 days at 4°C, and 38.2% after 7 days at 4°C, but was stable for 30 days at -20°C. Freezing urine samples is recommended for accurate analysis.
Journal of Analytical Toxicology
April 1, 2008
K. Bjornstad, A. Helander, O. Beck
20 citations
A liquid chromatography-tandem mass spectrometry (LC-MS-MS) method was developed to screen and confirm mescaline in human urine, with a detection limit of 3-5 micrograms per liter and an upper quantification limit of 10,000 micrograms per liter. The method proved sensitive and specific for routine testing. Among 462 urine samples from young people with alcohol or drug problems, 32% were positive for illicit drugs, but none for mescaline.
Journal of Analytical Toxicology
January 1, 2017
Adrian Stoller, Patrick C. Dolder, Michael Bodmer et al.
19 citations
A 19-year-old male was admitted to the emergency department with severe hallucinations, dilated pupils, rapid heart rate, agitation, and confusion after using a substance sold as 2C-B. Laboratory analysis using liquid chromatography-mass spectrometry detected the more potent synthetic phenethylamine derivative 2C-P instead. Based on two blood samples, the estimated elimination half-life was 19 hours. The case illustrates how small structural variations in the 4 position of the phenyl ring, such as a propyl group in 2C-P versus bromine in 2C-B, can lead to significant differences in drug potency and duration of action, contributing to adverse effects.
Journal of Analytical Toxicology
September 1, 2011
Sarah Kerrigan, Stephanie Banuelos, Laura Perrella et al.
19 citations
A gas chromatography–mass spectrometry method was developed to detect ten psychedelic phenethylamines (2C-B, 2C-H, 2C-I, 2C-T-2, 2C-T-7, 4-MTA, DOB, DOET, DOI, and DOM) in urine. After solid-phase extraction, limits of detection ranged from 2 to 10 ng/mL, and limits of quantitation were 10 ng/mL or less. Precision at 50 and 500 ng/mL gave coefficients of variation of 0.4–7.9%, and accuracy was 91–116%. Calibration curves were linear up to 1500 ng/mL. No carryover occurred at 5000 ng/mL, and no interferences from related compounds or endogenous bases were observed.