Journal of Analytical Toxicology
May 1, 1990
Damon I. Papac, Rodger L. Foltz
45 citations
A method originally developed to measure LSD in urine was adapted for use with plasma. After adding a deuterium-labeled version of LSD as an internal standard, the plasma is extracted and the drug is converted to a derivative for analysis by gas chromatography combined with negative ion chemical ionization mass spectrometry. The assay produced a linear response for concentrations between 0.1 and 3.0 ng/mL. When applied to a male volunteer who took 1 microgram of LSD per kilogram of body weight orally, the peak plasma concentration reached 1.9 ng/mL three hours after dosing, and the apparent plasma half-life was 5.1 hours.
Journal of Analytical Toxicology
January 1, 2003
Helena K. Nordgren, Olof Beck
43 citations
Liquid chromatography-tandem mass spectrometry (LC-MS-MS) with atmospheric pressure chemical ionization detected MDMA and MDA in urine with a 100 ng/mL cutoff and 10% coefficient of variation. In 1000 clinical patient urine samples, the LC-MS-MS method identified nearly four times as many MDMA-positive samples as the immunochemical method, with no false positives and one false negative. The findings suggest LC-MS-MS is a viable alternative to immunochemical screening for drugs of abuse.
Journal of Analytical Toxicology
July 1, 1985
Philip C. Reynolds, Ej Jindrich
43 citations
A fatal case involving mescaline intoxication is reported, with drug concentrations measured at 9.7 micrograms/mL in blood, 70.8 micrograms/g in liver, and 1163 micrograms/g in urine. These levels indicate a high degree of exposure and toxicity, contributing to the individual's death.
Journal of Analytical Toxicology
October 3, 2016
Eulàlia Olesti, Mitona Pujadas, Esther Papaseit et al.
41 citations
Mephedrone, a synthetic cathinone increasingly used by young people and linked to acute intoxication and fatalities, was studied in a controlled clinical trial. A gas chromatography-mass spectrometry method was developed to measure mephedrone in human plasma and urine. Six healthy men received 150 mg of mephedrone orally. Peak plasma concentration averaged 122.6 ng/mL, reached within 0.5–2 hours, and the drug was eliminated rapidly with a half-life of 2.2 hours. Less than 15% of the dose appeared unchanged in urine, and concentrations varied widely among individuals.
Journal of Analytical Toxicology
March 1, 2005
J. L. Villamor, Ana María Bermejo, María Pilar Murias Fernández et al.
40 citations
A new gas chromatography-mass spectrometry method allows simultaneous identification and measurement of five amphetamine-type drugs in hair. Hair samples are hydrolyzed in sodium hydroxide, extracted with a solvent mixture, and derivatized before analysis. The method is accurate to within ±9% and precise, with coefficients of variation below 8%. Detection limits range from 0.007 to 0.045 ng/mg depending on the drug. In 24 positive hair specimens, average concentrations were 0.88 ng/mg for amphetamine, 10.14 ng/mg for methamphetamine, 1.30 ng/mg for MDA, and 8.87 ng/mg for MDMA; only one specimen contained MDEA at 0.84 ng/mg.
Journal of Analytical Toxicology
March 1, 2004
Roman Stanaszek, Wojciech Piekoszewski
40 citations
A new analytical method using liquid chromatography with atmospheric-pressure chemical ionization mass spectrometry was developed to detect eight amphetamines in hair samples. After alkaline digestion and extraction, the method achieved detection limits as low as 0.05 ng/mg for methamphetamine, MDA, MDMA, and MDEA, and up to 0.20 ng/mg for methcathinone and PMA. Testing on 93 hair samples from patients in detoxification and methadone treatment found measurable concentrations of ephedrine, methcathinone, amphetamine, methamphetamine, MDMA, and MDEA, while MDA and PMA were never detected. The method provides a sensitive, linear response from 0 to 20 ng/mg for all target drugs.
Journal of Analytical Toxicology
May 1, 1990
Margaret M. Mccarron, Clifford B. Walberg, Randall C. Baselt
40 citations
Among 31 patients with suspected LSD intoxication, a radioimmunoassay (RIA) with a detection limit of 0.1 ng/mL identified LSD in 13 blood and urine specimens from 14 patients. High-performance liquid chromatography (HPLC) with a detection limit of 0.5 ng/mL confirmed LSD in 9 of 13 serum and 11 of 13 urine specimens that were RIA-positive. Of 18 patients ultimately diagnosed with LSD intoxication, RIA detected LSD in 14 and HPLC in 11. All 13 patients with other diagnoses had negative results by both methods. The authors conclude that a commercially available RIA provides reliable qualitative laboratory confirmation of LSD intoxication.
Journal of Analytical Toxicology
May 1, 2002
K. L. Klette, C. K. Horn, P. R. Stout et al.
39 citations
A major metabolite of LSD, 2-oxo-3-hydroxy lysergic acid diethylamide (O-H-LSD), is a superior marker for identifying LSD use because it appears in urine at concentrations 16 to 43 times higher than LSD itself. Testing a wide range of chemically similar compounds, over-the-counter products, prescription drugs, and other drugs of abuse showed none interfered with detecting O-H-LSD. The metabolite remained stable under refrigerated and frozen conditions within normal urine pH (4.6-8.4), but significant loss occurred at room temperature or higher (24-50°C). These findings support the forensic reliability of liquid chromatography-mass spectrometry for detecting LSD use via O-H-LSD.
Journal of Analytical Toxicology
October 1, 2000
K. L. Klette, Carolyn J. Anderson, Gregory K. Poch et al.
38 citations
The metabolism of LSD into a compound called O-H-LSD occurs in human liver cells. O-H-LSD is found in human urine at 16 to 43 times the concentration of LSD itself, and earlier work ruled out its formation during sample handling or storage. This study incubated human liver microsomes and hepatocytes with LSD and used liquid chromatography-mass spectrometry to analyze the products. O-H-LSD was positively identified in all samples treated with LSD but not in any controls. The results definitively show that O-H-LSD is produced as a metabolic product of LSD in human liver tissue.
Journal of Analytical Toxicology
September 1, 1999
Scott Reuschel, Shaundel Percey, S. Liu et al.
38 citations
A new assay can detect lysergic acid diethylamide (LSD) and its major metabolite, 2-oxo-3-hydroxy-LSD, in human urine at concentrations as low as 10 pg/mL. In most LSD-positive urine samples, the metabolite is present at higher concentrations than LSD and remains detectable longer after ingestion. The method uses solid-phase extraction, trimethylsilylation, and gas chromatography-tandem mass spectrometry with selected reaction monitoring. Linear calibration curves were obtained from 10 pg/mL to 5000 pg/mL. Reanalysis of 49 previously positive urine samples showed an average LSD concentration of 357 pg/mL and an average metabolite concentration of 3470 pg/mL. Clinical dosing experiments support that analyzing for the metabolite extends the detection window for identifying LSD use.
Journal of Analytical Toxicology
May 1, 2011
Jennifer L. Pilgrim, Dimitri Gerostamoulos, Olaf H. Drummer
36 citations
MDMA (ecstasy) is increasingly used and often combined with pharmaceutical drugs, especially serotonergic medications, raising concerns about toxicity and dangerous interactions. A review of all closed coronial cases in Victoria, Australia, from 2002 to 2008 identified 106 fatalities where MDMA was detected. Of these, 43 cases (41%) involved the concurrent use of MDMA with other drugs, including pharmaceuticals that could cause adverse reactions. Four cases were high-risk, involving the combination of MDMA and moclobemide, with additional moderate- and minor-risk cases. These findings underscore the need to recognize and publicize potentially lethal drug interactions, particularly serotonin toxicity.
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
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
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
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
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
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, 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, 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.