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Journal of Analytical Toxicology

ISSN 0146-4760

133 papers in the library · 4,317 citations · publishing 1977-2026

Papers

Fluorescence Polarization Immunoassay Detection of Amphetamine, Methamphetamine, and Illicit Amphetamine Analogues*

Journal of Analytical Toxicology January 1, 1993 John T. Cody, R H Schwarzhoff 54 citations

Two commercial immunoassay reagents, Abbott's Amphetamine/Methamphetamine II and Amphetamine Class, were tested for their ability to detect a wide range of amphetamine-related compounds, including stereoisomers, metabolites, and illicit analogues such as MDMA, MDA, and mescaline, at concentrations from 100 to 100,000 ng/mL. The Amphetamine/Methamphetamine II reagent showed better overall performance, especially for detecting over-the-counter medications, while the Amphetamine Class reagent did not improve detection of amphetamine, methamphetamine, or illicit analogues. Some illicit analogues were reliably detected, but many others were not. The Amphetamine Class reagents are a poor choice unless detecting over-the-counter compounds is specifically needed.

MDMA and MDA Concentrations in Antemortem and Postmortem Specimens in Fatalities Following Hospital Admission

Journal of Analytical Toxicology July 1, 2005 Simon Elliott 52 citations

MDMA and its metabolite MDA show postmortem redistribution, meaning concentrations measured after death are often higher than those taken just before death. In five hospital fatalities with both antemortem and postmortem blood samples, postmortem MDMA concentrations ranged from 0.47 to 28.39 mg/L compared to antemortem levels of 0.55 to 4.33 mg/L. Postmortem-to-antemortem ratios ranged from 1.1 to 6.6 for MDMA and 1.5 to 13.3 for MDA. Central sites like the heart had much higher concentrations than peripheral sites like the femoral vein. Thus, postmortem blood levels, even from peripheral sites, are not directly comparable to antemortem findings near death.

Matrix Effect and Cross-Reactivity of Select Amphetamine-Type Substances, Designer Analogues, and Putrefactive Amines using the Bio-Quant Direct ELISA Presumptive Assays for Amphetamine and Methamphetamine

Journal of Analytical Toxicology May 1, 2007 Luigino G. Apollonio, Ian R. Whittall, Dennis J. Pianca et al. 51 citations

Bio-Quant Direct ELISA kits for amphetamine and methamphetamine can reliably detect these drugs in blood, urine, and saliva down to 3 ng/mL in buffer and 6 ng/mL in biological matrices. The amphetamine kit also detects MDA (282% cross-reactivity), PMA (265%), 4-MTA (280%), and phentermine (61%). The methamphetamine kit cross-reacts with MDMA (73%), MDEA (18%), pseudoephedrine (19%), MBDB (8%), and ephedrine (9%). Both kits are fast and accurate for routine toxicological screening.

The Detection of Novel Stimulants in Oral Fluid from Users Reporting Ecstasy, Molly and MDMA Ingestion

Journal of Analytical Toxicology July 16, 2018 Alex J. Krotulski, Amanda L A Mohr, Melissa F. Fogarty et al. 50 citations

Among people attending electronic dance music festivals, self-reported use of Ecstasy, Molly, or MDMA often does not match what is actually in their system. Over four years, oral fluid from 223 participants who said they had recently used one or more of those terms was tested. Only 54.3% had MDMA alone; 29.6% tested positive for a novel stimulant instead. Most participants (91%) used only one term, with Molly the most common (60.6%), followed by MDMA (27.1%) and Ecstasy (12.3%). The findings indicate that the terms Ecstasy, Molly, and MDMA are not used interchangeably or accurately, and that users may unknowingly consume novel psychoactive substances.

Sweat Testing of MDMA with the Drugwipe(R) Analytical Device: A Controlled Study with Two Volunteers

Journal of Analytical Toxicology March 1, 2001 Roberta Pacifici, Magı́ Farré, Simona Pichini et al. 50 citations

After a single 100 mg oral dose of MDMA, the Drugwipe immunochemical strip test detected the drug in sweat from two volunteers as early as 2 hours and up to 12 hours later. However, one volunteer showed a faint positive result before dosing, when plasma and urine were negative, and this persisted beyond 48 hours. Gas chromatography-mass spectrometry measured peak plasma concentrations of MDMA and its metabolite HMMA at 2-4 hours, with levels above 20 ng/mL and 40 ng/mL respectively still present at 24 hours. Urine remained positive for both substances over 48 hours. These results suggest sweat testing with Drugwipe may be useful for monitoring MDMA use.

Stability Study of LSD Under Various Storage Conditions

Journal of Analytical Toxicology October 1, 1998 Zhi Li, A. J. Mcnally, Honggang Wang et al. 50 citations

LSD in pooled urine is stable for up to 4 weeks at 25 degrees C in the dark, with no significant loss. At 37 degrees C, a 30% loss occurred after 4 weeks, and up to 40% at 45 degrees C. Amber glass or nontransparent polyethylene containers preserved LSD concentration under any light conditions; stability in transparent containers depended on distance from light source, wavelength, exposure time, and intensity. Prolonged heat in alkaline pH converted 10 to 15% of LSD to iso-LSD; under acidic conditions, less than 5% converted. Trace metal ions catalyzed decomposition, preventable by adding EDTA. Proper storage is essential for accurate analytical testing.

MDA-MDMA Concentrations in Urine Specimens*

Journal of Analytical Toxicology November 1, 1996 Gary W. Kunsman, Barry Levine, James J. Kuhlman et al. 48 citations

Urine specimens from 34 active-duty U.S. Army personnel who tested positive for amphetamines were reanalyzed. All samples contained both MDMA (ecstasy) and its metabolite MDA. MDMA concentrations ranged from 0.38 to 96.2 mg/L (mean 13.4 mg/L), and MDA concentrations ranged from 0.15 to 8.6 mg/L (mean 1.6 mg/L). The average ratio of MDA to MDMA was 0.15, similar to the ratio of amphetamine to methamphetamine (0.10). The presence of MDA at about 10–15% of the MDMA concentration is consistent with MDMA metabolism alone, suggesting use of only MDMA rather than combined use of both drugs.

Liquid chromatography-tandem mass spectrometry method for the simultaneous analysis of multiple hallucinogens, chlorpheniramine, ketamine, ritalinic acid, and metabolites, in urine.

Journal of Analytical Toxicology October 1, 2007 Maria Del Mar Ramirez Fernandez, Marleen Laloup, Michelle Wood et al. 47 citations

A method for simultaneously measuring multiple hallucinogens, chlorpheniramine, ketamine, ritalinic acid, and several metabolites in human urine was developed and validated. The procedure uses solid-phase extraction followed by liquid chromatography-tandem mass spectrometry, with all drugs eluting within 14 minutes. Using 500 microliters of urine, limits of quantification ranged from 0.05 ng/mL for LSD to 10 ng/mL for other hallucinogens, with linear or quadratic regression from each compound's limit up to 500 ng/mL. Precision and accuracy were acceptable, and processed samples remained stable in the autosampler for at least 24 hours. The method was successfully applied to authentic urine samples containing chlorpheniramine, ketamine, LSD, and psilocin.

Distribution Study of 3,4-Methylenedioxymethamphetamine and 3,4-Methylenedioxyamphetamine in a Fatal Overdose

Journal of Analytical Toxicology March 1, 2002 Els A. de Letter, Karine M. Clauwaert, Willy E. Lambert et al. 47 citations

In a fatal overdose of MDMA (ecstasy) and its metabolite MDA, concentrations varied widely across different body sites. Central blood samples (heart and great vessels) showed different levels than peripheral blood (subclavian and femoral). High levels were found in liver, lungs, and kidneys, while vitreous humor also contained MDMA, suggesting it could be used when blood is unavailable. The findings confirm that peripheral vein blood is best for accurate measurement, and that postmortem redistribution must be considered when interpreting toxicology results from other sites.

Enantiomeric Separation and Quantitation of ( )-Amphetamine, ( )-Methamphetamine, ( )-MDA, ( )-MDMA, and ( )-MDEA in Urine Specimens by GC-EI-MS after Derivatization with (R)-(-)- or (S)-(+)- -Methoxy- -(trifluoromethy)phenylacetyl Chloride (MTPA)

Journal of Analytical Toxicology September 1, 2004 Bindu D. Paul, John F. Jemionek, David Lesser et al. 46 citations

A new gas chromatography-mass spectrometry (GC-MS) method using (R)-(-)-alpha-methoxy-alpha-(trifluoromethyl)phenylacetyl chloride (MTPA) as a chiral derivatizing agent avoids racemization problems seen with the standard reagent (S)-(-)-trifluoroacetylprolyl chloride (TPC). The MTPA method reliably separates the (R)-(-)- and (S)-(+)-isomers of methamphetamine, amphetamine, MDA, MDMA, and MDEA. In 91% of methamphetamine-positive urine specimens, only the (S)-(+)-isomer—indicative of illicit use—was detected. For MDMA-positive specimens, (R)-(-)-isomer concentrations exceeded (S)-(+)-isomer, suggesting longer bodily retention of the (R)-(-)-form. Quantitation was linear over 25–10,000 ng/mL for most drugs, with correlation coefficients >0.996 and precision within ±11% at 500 ng/mL. The single MTPA method can replace two separate GC-MS tests needed to confirm illicit (S)-(+)-amphetamine and methamphetamine use.

Measurement of Lysergic Acid Diethylamide (LSD) in Human Plasma by Gas Chromatography/Negative Ion Chemical Ionization Mass Spectrometry*

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.

Identification and quantitation of ibogaine and an o-demethylated metabolite in brain and biological fluids using gas chromatography-mass spectrometry.

Journal of Analytical Toxicology October 1, 1995 W L Hearn, J Pablo, G W Hime et al. 44 citations

A sensitive method was developed to measure ibogaine and its major metabolite, 12-hydroxy-ibogamine (noribogaine), in biological fluids and brain tissue. The metabolite was identified using gas chromatography-mass spectrometry. The procedure involves solvent extraction, derivatization with ethyl iodide, and cleanup before analysis. Detection limits were 5 ng/mL for both compounds, and quantitation limits ranged from 5 to 10 ng/mL across all tested matrices. Calibration curves were linear from 3 to 1000 ng/mL or ng/g.

Direct Screening of Urine for MDMA and MDA by Liquid Chromatography-Tandem Mass Spectrometry*

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.

GC–MS Quantification Method for Mephedrone in Plasma and Urine: Application to Human Pharmacokinetics

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.

Gas Chromatography-Mass Spectrometry Method for the Quantitative Identification of 23 New Psychoactive Substances in Blood and Urine.

Journal of Analytical Toxicology June 1, 2019 Lorna A. Nisbet, Fiona M Wylie, Barry K. Logan et al. 40 citations

A validated gas chromatography-mass spectrometry (GC-MS) method can simultaneously quantify 23 new psychoactive substances (NPSs) in blood and urine, including NBOMe compounds that are usually analyzed by liquid chromatography-tandem mass spectrometry. The method, which uses solid-phase extraction and derivatization, met SWGTOX guidelines for bias, precision, linearity, and stability. When applied to reanalyze 12 blood samples from eight cases where 25I-NBOMe, 25C-NBOMe, methoxetamine, and methylone had previously been detected, the method quantitatively detected these drugs in 75% of samples, with 42% containing either 25C-NBOMe or 25I-NBOMe. This approach offers a practical alternative for laboratories lacking specialized equipment.

A New GC-MS Method for the Determination of Five Amphetamines in Human Hair

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.

Simultaneous Determination of Eight Underivatized Amphetamines in Hair by High-Performance Liquid Chromatography-Atmospheric Pressure Chemical Ionization Mass Spectrometry (HPLC-APCI-MS)

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.

Confirmation of LSD Intoxication by Analysis of Serum and Urine

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.

LC-MS Analysis of Human Urine Specimens for 2-Oxo-3-Hydroxy LSD: Method Validation for Potential Interferants and Stability Study of 2-Oxo-3-Hydroxy LSD Under Various Storage Conditions

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.

Four fatalities involving 5-IT.

Journal of Analytical Toxicology September 1, 2013 L Nitin Seetohul, Derrick J. Pounder 38 citations

Four deaths are associated with the new designer stimulant 5-(2-aminopropyl)indole (5-IT), an indole derivative first synthesized in 1962. In three cases, 5-IT was detected in femoral blood at concentrations ranging from 0.4 to 10 mg/L, often alongside other drugs such as MDMA, 6-APB, amphetamine, and methylone. One death was attributed solely to 5-IT toxicity; two deaths were attributed to toxic cocktail effects of multiple drugs; and one death was attributed to drug toxicity with an indeterminate role of epilepsy. A validated high-performance liquid chromatography method for quantitating 5-IT is also reported.

Distribution of ibogaine and noribogaine in a man following a poisoning involving root bark of the Tabernanthe iboga shrub.

Journal of Analytical Toxicology September 1, 2006 Violeta Kontrimaviciūte, Olivier Mathieu, Jean-Claude Mathieu-Daudé et al. 38 citations

In a 48-year-old Caucasian male with a history of drug abuse who died after ingesting root bark from the shrub Tabernanthe iboga, ibogaine and its main metabolite noribogaine were found in all examined tissues except cardiac tissue. The highest concentrations appeared in spleen, liver, brain, and lung. Tissue-to-blood concentration ratios for ibogaine averaged 1.78 in spleen, 3.75 in liver, 1.16 in brain, and 4.64 in lung; for noribogaine, the ratios were 0.83, 2.43, 0.90, and 2.69, respectively. Both substances crossed the blood-brain barrier and were secreted in bile. Very low concentrations occurred in prostatic tissue.

Metabolism of Lysergic Acid Diethylamide (LSD) to 2-Oxo-3-Hydroxy LSD (O-H-LSD)in Human Liver Microsomes and Cryopreserved Human Hepatocytes

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.

Quantitative Determination of LSD and a Major Metabolite, 2-Oxo-3-Hydroxy-LSD, in Human Urine by Solid-Phase Extraction and Gas Chromatography-Tandem Mass Spectrometry

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.

Deaths Involving MDMA and the Concomitant Use of Pharmaceutical Drugs

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.