Detection of ketamine and its metabolites in urine by ultra high pressure liquid chromatography-tandem mass spectrometry

Mark C. Parkin, Sophie C. Turfus, Norman W. Smith, John M. Halket, Robin A. Braithwaite, Simon P. Elliott, M. David Osselton, David A. Cowan, Andrew T. Kicman

Research output: Contribution to journalArticle

68 Citations (Scopus)

Abstract

Current analytical methods used for screening drugs and their metabolites in biological samples from victims of drug-facilitated sexual assault (DFSA) or other vulnerable groups can lack sufficient sensitivity. The application of liquid chromatography, employing small particle sizes, with tandem mass spectrometry (MS/MS) is likely to offer the sensitivity required for detecting candidate drugs and/or their metabolites in urine, as demonstrated here for ketamine. Ultra-performance liquid chromatography-mass spectrometry (UPLC-MS/MS) was performed following extraction of urine (4 mL) using mixed-mode (cation and C8) solid-phase cartridges. Only 20 μL of the 250 μL extract was injected, leaving sufficient volume for other assays important in DFSA cases. Three ion transitions were chosen for confirmatory purposes. As ketamine and norketamine (including their stable isotopes) are available as reference standards, the assay was additionally validated for quantification purposes to study elimination of the drug and primary metabolite following a small oral dose of ketamine (50 mg) in 6 volunteers. Dehydronorketamine, a secondary metabolite, was also analyzed qualitatively to determine whether monitoring could improve retrospective detection of administration. The detection limit for ketamine and norketamine was 0.03 ng/mL and 0.05 ng/mL, respectively, and these compounds could be confirmed in urine for up to 5 and 6 days, respectively. Dehydronorketamine was confirmed up to 10 days, providing a very broad window of detection.

LanguageEnglish
Pages137-142
Number of pages6
JournalJournal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences
Volume876
Issue number1
DOIs
Publication statusPublished - 1 Dec 2008
Externally publishedYes

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High pressure liquid chromatography
Ketamine
Metabolites
Tandem Mass Spectrometry
Mass spectrometry
High Pressure Liquid Chromatography
Urine
Liquid Chromatography
Pharmaceutical Preparations
Liquid chromatography
Assays
Preclinical Drug Evaluations
Particle Size
Isotopes
Limit of Detection
Cations
Volunteers
Mass Spectrometry
Ions
Screening

Cite this

Parkin, Mark C. ; Turfus, Sophie C. ; Smith, Norman W. ; Halket, John M. ; Braithwaite, Robin A. ; Elliott, Simon P. ; Osselton, M. David ; Cowan, David A. ; Kicman, Andrew T. / Detection of ketamine and its metabolites in urine by ultra high pressure liquid chromatography-tandem mass spectrometry. In: Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences. 2008 ; Vol. 876, No. 1. pp. 137-142.
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Detection of ketamine and its metabolites in urine by ultra high pressure liquid chromatography-tandem mass spectrometry. / Parkin, Mark C.; Turfus, Sophie C.; Smith, Norman W.; Halket, John M.; Braithwaite, Robin A.; Elliott, Simon P.; Osselton, M. David; Cowan, David A.; Kicman, Andrew T.

In: Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences, Vol. 876, No. 1, 01.12.2008, p. 137-142.

Research output: Contribution to journalArticle

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AU - Parkin, Mark C.

AU - Turfus, Sophie C.

AU - Smith, Norman W.

AU - Halket, John M.

AU - Braithwaite, Robin A.

AU - Elliott, Simon P.

AU - Osselton, M. David

AU - Cowan, David A.

AU - Kicman, Andrew T.

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