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Quantitation of the...
Quantitation of the enantiomers of tramadol and its three main metabolites in human whole blood using LC-MS/MS.
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- Haage, Pernilla (författare)
- Linköpings universitet,Avdelningen för läkemedelsforskning,Medicinska fakulteten,National Board of Forensic Medicine, Department of Forensic Genetics and Forensic Toxicology, Linköping Sweden
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- Kronstrand, Robert (författare)
- Linköpings universitet,Avdelningen för läkemedelsforskning,Medicinska fakulteten,National Board of Forensic Medicine, Department of Forensic Genetics and Forensic Toxicology, Linköping Sweden
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- Carlsson, Björn (författare)
- Linköpings universitet,Avdelningen för läkemedelsforskning,Medicinska fakulteten,Region Östergötland, Klinisk farmakologi
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- Josefsson, Martin (författare)
- Linköpings universitet,Institutionen för fysik, kemi och biologi,Tekniska fakulteten,National Board of Forensic Medicine, Department of Forensic Genetics and Forensic Toxicology, Linköping Sweden
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(creator_code:org_t)
- Elsevier BV, 2016
- 2016
- Engelska.
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Ingår i: Journal of Pharmaceutical and Biomedical Analysis. - : Elsevier BV. - 0731-7085 .- 1873-264X. ; 119, s. 1-9
- Relaterad länk:
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https://urn.kb.se/re...
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https://doi.org/10.1...
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Abstract
Ämnesord
Stäng
- The analgesic drug tramadol and its metabolites are chiral compounds, with the (+)- and (-)-enantiomers showing different pharmacological and toxicological effects. This novel enantioselective method, based on LC-MS/MS in reversed phase mode, enabled measurement of the parent compound and its three main metabolites O-desmethyltramadol, N-desmethyltramadol and N,O-didesmethyltramadol simultaneously. Whole blood samples of 0.5g were fortified with internal standards (tramadol-(13)C-D3 and O-desmethyl-cis-tramadol-D6) and extracted under basic conditions (pH 11) by liquid-liquid extraction. Chromatography was performed on a chiral alpha-1-acid glycoprotein (AGP) column preceded by an AGP guard column. The mobile phase consisted of 0.8% acetonitrile and 99.2% ammonium acetate (20mM, pH 7.2). A post-column infusion with 0.05% formic acid in acetonitrile was used to enhance sensitivity. Quantitation as well as enantiomeric ratio measurements were covered by quality controls. Validation parameters for all eight enantiomers included selectivity (high), matrix effects (no ion suppression/enhancement), calibration model (linear, weight 1/X(2), in the range of 0.25-250ng/g), limit of quantitation (0.125-0.50ng/g), repeatability (2-6%) and intermediate precision (2-7%), accuracy (83-114%), dilution integrity (98-115%), carry over (not exceeding 0.07%) and stability (stable in blood and extract). The method was applied to blood samples from a healthy volunteer administrated a single 100mg dose and to a case sample concerning an impaired driver, which confirmed its applicability in human pharmacokinetic studies as well as in toxicological and forensic investigations.
Ämnesord
- NATURVETENSKAP -- Kemi -- Analytisk kemi (hsv//swe)
- NATURAL SCIENCES -- Chemical Sciences -- Analytical Chemistry (hsv//eng)
Nyckelord
- Enantiomer; LC–MS/MS; N
- O-didesmethyltramadol; N-desmethyltramadol; O-desmethyltramadol; Tramadol
Publikations- och innehållstyp
- ref (ämneskategori)
- art (ämneskategori)
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