Development and validation of an LC–MS/MS method for the quantification of ephedrines in urine

Deventer, Koen; Pozo, Óscar J.; Eenoo, Peter Van; Delbeke, Frans

doi:10.1016/j.jchromb.2008.12.032

Cited by 53 publications

(33 citation statements)

References 18 publications

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“…Some ions resulting from neutral losses of water and a methyl group are common for similar molecules, such as amphetamine and ephedrine derivatives (Deventer et al, 2009;Bijlsma et al, 2011). However, the observed MS/MS behavior of mephedrone was to some extent unexpected.…”

Section: Mass Spectrometric Behavior Of Mephedronementioning

confidence: 99%

“…However, the observed MS/MS behavior of mephedrone was to some extent unexpected. Nitrogen-containing stimulants usually lose the amine group (normally as ammonia or methylamine) in one of the first fragmentation steps (Deventer et al, 2009;Bijlsma et al, 2011). Contrary to this behavior, the neutral loss of methylamine is poor (2%; see Table 1) for mephedrone.…”

Section: Mass Spectrometric Behavior Of Mephedronementioning

confidence: 99%

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Mass Spectrometric Evaluation of Mephedrone In Vivo Human Metabolism: Identification of Phase I and Phase II Metabolites, Including a Novel Succinyl Conjugate

Pozo

Ibáñez

Sancho

et al. 2015

Drug Metabolism and Disposition

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In recent years, many new designer drugs have emerged, including the group of cathinone derivatives. One frequently occurring drug is mephedrone; although mephedrone was originally considered as a "legal high" product, it is currently banned in most Western countries. Despite the banning, abuse of the drug and seizures are continuously reported. Although the metabolism of mephedrone has been studied in rats or in vitro using human liver microsomes, to the best of our knowledge, no dedicated study with human volunteers has been performed for studying the in vivo metabolism of mephedrone in humans. Therefore, the aim of this study was to establish the actual human metabolism of mephedrone and to compare it with other models. For this purpose, urine samples of two healthy volunteers, who ingested 200 mg mephedrone orally, were taken before administration and 4 hours after substance intake. The discovery and identification of the phase I and phase II metabolites of mephedrone were based on ultra-high-performance liquid chromatography coupled to hybrid quadrupole time-of-flight mass spectrometry, operating in the so-called MS E mode. Six phase I metabolites and four phase II metabolites were identified, four of them not previously reported in the literature. The structure of four of the detected metabolites was confirmed by synthesis of the suggested compounds. Remarkably, a mephedrone metabolite conjugated with succinic acid has been identified and confirmed by synthesis. According to the reviewed literature, this is the first time that this type of conjugate is reported for human metabolism.

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Section: Mass Spectrometric Behavior Of Mephedronementioning

confidence: 99%

Section: Mass Spectrometric Behavior Of Mephedronementioning

confidence: 99%

Mass Spectrometric Evaluation of Mephedrone In Vivo Human Metabolism: Identification of Phase I and Phase II Metabolites, Including a Novel Succinyl Conjugate

Pozo

Ibáñez

Sancho

et al. 2015

Drug Metabolism and Disposition

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“…[82] In another analytical work a quantitative LC-MS/MS method was developed for the detection of ephedrines in diluted urine samples and compared to the traditional GC/NPD method. [83] Another research group examined the possibility of exceeding the urinary ephedrine thresholds when administering Chinese herbal preparations Sho-seiryu-to [84] and Kakkon-to. [85] The conclusion of these studies was that the risk is not high with a single dose of the preparations, but is exceeded when the administration period is longer and multiple doses are consumed.…”

Section: Stimulantsmentioning

confidence: 99%

Annual banned‐substance review: analytical approaches in human sports drug testing

Thevis

Kuuranne

Geyer

et al. 2010

Drug Testing and Analysis

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“…11 Among them, LC-MS/MS is the most frequently used method, enabling the direct injection of dilute urine into the chromatographic system. This approach is very straightforward, simple and quick, and decreases sample handling and improves the robustness of quantification.…”

Section: Introductionmentioning

confidence: 99%

Fast Ephedrine Quantification by Gas Chromatography Mass Spectrometry

Carneiro¹,

Silva²,

Cavalcante³

et al. 2018

J. Braz. Chem. Soc.

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Ephedrines are widely used in therapy. Because of their stimulant properties, these substances are relevant in different forensic fields. At present, the state of the art for ephedrines quantification relay based on a liquid chromatography mass spectrometry, mainly because of the dilute-andshoot approach. Notwithstanding, several gas chromatography based methods have already been described, all of them include cleanup steps, with the potential disadvantage of incurring errors and increasing the workload. In this paper, a straightforward method for ephedrine quantification based on gas chromatographic mass spectrometry, without cleanup and based on Doehlert matrix optimization is presented. Only 10 µL of a urine sample is necessary and for N-methyl-N-(trimethylsilyl)trifluoroacetamide/N-methyl-bis-trifluoracetamide derivatives, the intermediate precision was 2.77% for ephedrine, 9.20% for cathine, 8.29% for norephedrine and 4.27% for pseudoephedrine. The limit of detection was 20 ng mL -1 for ephedrine, 30 ng mL -1 for cathine and 40 ng mL -1 for norephedrine and pseudoephedrine.

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Development and validation of an LC–MS/MS method for the quantification of ephedrines in urine

Cited by 53 publications

References 18 publications

Mass Spectrometric Evaluation of Mephedrone In Vivo Human Metabolism: Identification of Phase I and Phase II Metabolites, Including a Novel Succinyl Conjugate

Mass Spectrometric Evaluation of Mephedrone In Vivo Human Metabolism: Identification of Phase I and Phase II Metabolites, Including a Novel Succinyl Conjugate

Annual banned‐substance review: analytical approaches in human sports drug testing

Fast Ephedrine Quantification by Gas Chromatography Mass Spectrometry

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