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See detailIdentification and structure elucidation of four cannabimimetic compounds in seized products
Denooz, Raphaël ULg; VAN HEUGEN, Jean-Claude ULg; Frederich, Michel ULg et al

in Journal of Analytical Toxicology (2013), 37(2), 56-63

Since 2008, herbal mixtures with synthetic cannabinoid compounds have been sold as incense throughout the world. Although these new drugs are labeled as not for human consumption, these products are ... [more ▼]

Since 2008, herbal mixtures with synthetic cannabinoid compounds have been sold as incense throughout the world. Although these new drugs are labeled as not for human consumption, these products are smoked for their cannabis-like effects. This study reports the structural and spectral elucidation of four cannabimimetic compounds seized in Belgium: (4-methoxyphenyl)-1-(pentyl-1H-indol-3-yl)methanone (RCS-4), 1-(5-fluoropentyl)-3-(1-naphtoyl)indole (AM-2201), 2-(2-chlorophenyl)-1-(1-pentylindol-3-yl)ethanone (JWH-203) and 4-ethylnaphthalen-1-yl-(1-pentylindol-3-yl)methanone (JWH-210). Laboratory investigations were conducted by liquid chromatography (LC)–ultraviolet spectroscopy, high-resolution accurate mass detection and nuclear magnetic resonance (NMR) analysis. This combined analytical approach allowed the detection of illicit compounds for which reference materials were not available. To facilitate identification and to complete existing databases, ultraviolet spectra and NMR data of all seized products are presented. Additionally, LC–quadrupole time-of-flight data were recorded to provide absolute identification. [less ▲]

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See detailValidation of the quantitative determination of tetrahydrocannabinol and its two major metabolites in plasma by UHPLC/MS-MS according to the total error approach
DUBOIS, Nathalie ULg; Paccau, A.; DE BACKER, Benjamin ULg et al

in Journal of Analytical Toxicology (2012), 36(1), 25-29

In Belgium, driving under the influence (DUI) of cannabis is prohibited and has severe legal consequences for the driver if the blood plasma concentration of Δ9-tetrahydrocannabinol (THC) exceeds 1 µg/L ... [more ▼]

In Belgium, driving under the influence (DUI) of cannabis is prohibited and has severe legal consequences for the driver if the blood plasma concentration of Δ9-tetrahydrocannabinol (THC) exceeds 1 µg/L. A method to quantify low concentrations of THC and its hydroxylated (THC-OH) and carboxylated (THC-COOH) metabolites in plasma was developed for DUI but also for other applications. Ultra-high-performance liquid chromatography coupled to mass spectrometry seems to be a very convenient method to combine fast chromatographic separation and good sensitivity. The method was validated according to total error approach. Chromatographic separation was achieved in a 3-min total run time. The limits of quantitation were lower or equal to 1 µg/L for all compounds. The linearity of the method was acceptable in the validated range of concentrations (from 0.5 to 50 µg/L for THC, from 0.9 to 50 µg/L for THC-OH and from 1.1 to 100 µg/L for THC-COOH). The biases were lower than 13%, and the relative standard deviations for repeatability and intermediate precision did not exceed 15%. Lower and upper β-expectation tolerance limits did not exceed the acceptance limits of 20% for concentrations higher than 2 µg/L for THC and THC-OH and higher than 4 µg/L for THC-COOH. The acceptance limits were 30% for THC and THC-OH concentrations lower than 2 µg/L and for THC-COOH concentrations lower than 4 µg/L. [less ▲]

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See detailBlood, urine, and hair kinetic analysis following an acute lead intoxication
Ho, Thi Thanh Giang ULg; KEUTGENS, Aurore ULg; SCHOOFS, Roland et al

in Journal of Analytical Toxicology (2011), 35(1), 60-64

A case of lead exposure resulting from the accidental ingestion of a lead-containing solution is reported. Because of clinical management rapidly performed through chelation therapy by 2,3 ... [more ▼]

A case of lead exposure resulting from the accidental ingestion of a lead-containing solution is reported. Because of clinical management rapidly performed through chelation therapy by 2,3-dimercaptopropane sulfonate sodium and meso-2,3-dimercaptosuccinic acid, blood lead levels of this 51-year-old patient were moderate (412.9 μg/L) and no clinical symptoms were observed. Numerous blood and urine samples were collected for kinetic analysis of lead elimination. However, we report the first case in which hair samples were analyzed to determine the excretion level of lead after acute intoxication. [less ▲]

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See detailQuantification in postmortem blood and identification in urine of tramadol and its two main metabolites in two cases of lethal tramadol intoxication
De Backer, Benjamin ULg; Renardy, Françoise ULg; Denooz, Raphaël ULg et al

in Journal of Analytical Toxicology (2010), 34(9), 599-604

Tramadol has been extensively prescribed for two decades. It is an opioid analgesic considered to induce fewer side effects than other compounds of this class. However, serious complications may occur in ... [more ▼]

Tramadol has been extensively prescribed for two decades. It is an opioid analgesic considered to induce fewer side effects than other compounds of this class. However, serious complications may occur in case of intoxication. We report here two cases of fatal intoxication due to tramadol ingestion. Tramadol, O-desmethyltramadol (ODT) and N-desmethyltramadol (NDT) were quantitatively and qualitatively determined in postmortem blood and urine, respectively. An HPLC method coupled with fluorescence detection was validated using total error approach for the analysis of tramadol, ODT, and NDT in blood. In case1, concentrations of tramadol and its metabolites were 7.7 mg/L (tramadol), 1.33 mg/L (ODT), and 0.6mg/L (NDT). In case 2, concentrations found were 48.34 mg/L (tramadol), 2.43 mg/L (ODT), and 10.09 mg/L (NDT). Opposite ratios of ODT/NDT concentrations observed in different cases were suggested to be useful for the evaluation of the delay between ingestion and death. However, the changes in metabolites levels may also be explained by pharmacokinetic interactions and quantitative differences in the activity of the cytochrome-P450 2D6. Interestingly, norfluoxetine was detected in sub-therapeutic levels in case 2. Most of these aspects in tramadol-related fatalities are reviewed in this paper, and an overview of fatal intoxications due to tramadol is presented. [less ▲]

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See detailUPLC MS/MS method for the determination of bupropion and its main metabolites in human whole blood
Denooz, Raphael ULg; Mercerolle, M.; Lachatre, C. et al

in Journal of Analytical Toxicology (2010), 34(5), 280-286

A selective and sensitive ultra-performance liquid chromatography (UPLC)–electrospray ionization-tandem mass spectrometry (MS) method for simultaneous determination of bupropion and its main metabolites ... [more ▼]

A selective and sensitive ultra-performance liquid chromatography (UPLC)–electrospray ionization-tandem mass spectrometry (MS) method for simultaneous determination of bupropion and its main metabolites, hydroxybupropion, erythrohydrobupropion, and threohydrobupropion, in human whole blood is presented. The sample preparation consists of cleanup protein precipitation with methanol combined with a solid-phase extraction on Oasis HLB cartridges. Analytes were separated on a Waters Acquity UPLC® BEH phenyl column using a binary mobile phase consisting of ammonium formate buffer (2 mM, pH 4) and acetonitrile. Detection was performed on a Waters Acquity UPLC system coupled to a Quattro Premier triple-quadrupole MS in positive ion selected reaction monitoring. Internal standards were bupropion-d9 and hydroxybupropion-d6. Linearity was from 5 to 1000 ng/mL for bupropion and from 10 to 2000 ng/mL for metabolites. Accuracy profiles (80–120%), precision (< 15%), and limits of detection (1 ng/mL for bupropion and 2 ng/mL for metabolites) were also evaluated and responded to all criteria of validation. The aim of this study was to compare this presented method with a previously described method developed on a classic liquid chromatography–tandem MS system. [less ▲]

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See detailA fatal case of bupropion (ZybanR) overdose
Mercerolle, Magali; Denooz, Raphael ULg; Lachâtre, Gérard et al

in Journal of Analytical Toxicology (2008), 32

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See detailFatal overdosage with cisplatin
Charlier, Corinne ULg; Kintz, Pascal; Dubois, Nathalie ULg et al

in Journal of Analytical Toxicology (2004), 28(2), 138-140

This paper presents a case of fatal overdosage due to an accidental massive administration (750 mg instead of 170 mg) of cisplatin, an anticancer agent, to a 63-year-old patient suffering from lymphoma ... [more ▼]

This paper presents a case of fatal overdosage due to an accidental massive administration (750 mg instead of 170 mg) of cisplatin, an anticancer agent, to a 63-year-old patient suffering from lymphoma. Platinum was measured in various postmortem samples by means of inductively coupled plasma mass spectrometry. Heart and peripheral blood concentrations of platinum were 1515 and 1253 micro g/L, respectively. Concentrations in urine and bile were 1038 and 501 micro g/L, respectively. Renal dialysis was started immediately after the end of cisplatin perfusion, when the mistake was noticed, but the patient deceased at day 16, presenting renal and hepatic insufficiency, ototoxicity, and pancytopenia. [less ▲]

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See detailAnalysis of polychlorinated biphenyl residues in human plasma by gas chromatography-mass spectrometry
Charlier, Corinne ULg; Dubois, Nathalie ULg; Cucchiaro, Sabine ULg et al

in Journal of Analytical Toxicology (2003), 27(2), 74-77

A method for the determination of seven polychlorinated biphenyl residues in plasma by gas chromatography-mass spectrometry was developed. The analytes were isolated from human plasma by liquid-liquid ... [more ▼]

A method for the determination of seven polychlorinated biphenyl residues in plasma by gas chromatography-mass spectrometry was developed. The analytes were isolated from human plasma by liquid-liquid extraction, followed by solid-phase extraction, and separation on an HP5 Trace column. Ionization mode was electronic impact, and selected ion storage was used for isolation and quantitation of the compounds. The method was evaluated for its analytical performances and therefore applied to monitor the prevalence of these seven polychlorinated biphenyl residues in a female population. Eighty samples were analyzed, and 82.5% presented detectable amounts of at least one residue. For the population study, results were reported on a lipid-adjusted basis. Because the proposed method is satisfying and seems to be suitable for the quantitation of PCB congeners in a general population, epidemiological studies to evaluate the widespread contamination with these environmental compounds can be proposed. [less ▲]

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