title: Enatiomeric determination of tramadol and O-desmethyltramadol in human urine by gas chromatography-mass spectrometry.
abstract: A GC-MS assay for stereoselective determination of tramadol and its pharmacologically active phase I metabolite O-desmethyltramadol in human urine was developed. Nefopam was used as internal standard. The method involves a simple solid phase extraction with chiral analysis by gas chromatography-electron ionization mass spectrometry using m/z 263; 58, 249; 58, and 179; 58 for the determination of concentration of tramadol, O-desmethyltramadol and internal standard, respectively. Chromatography was performed on a Rt-betaDEXcst column containing alkylated beta-cyclodextrins as a chiral selector. The calibration curves were linear in the concentration range 0.1-20 microg/mL (R(2) > or =0.998). Intra-day accuracies ranged between 97.2-104.9%, 96.1-103.2%, and 97.3-102.8% at the lower, intermediate, and high concentration for all analytes, respectively. Inter-day accuracies ranged between 95.2-105.7%, 99.1-105.2%, and 96.5-101.2% at the lower, intermediate, and high concentration for all analytes, respectively. This method was successfully used to determine the concentration of enantiomers of T and ODT in a pharmacogenetic study.
authors.affiliation: Institute of Forensic Medicine and Toxicology, 1st Faculty of Medicine, Charles University in Prague, 12108 Prague 2, Czech Republic. lukas.chytil@lf1.cuni.cz
authors.forename: Lukás
authors.initials: L
authors.lastname: Chytil
authors.forename: Martin
authors.initials: M
authors.lastname: Stícha
authors.forename: Olga
authors.initials: O
authors.lastname: Matousková
authors.forename: Frantisek
authors.initials: F
authors.lastname: Perlík
authors.forename: Ondrej
authors.initials: O
authors.lastname: Slanar
mesh_terms: D000701:Analgesics, Opioid / Q000737:chemistry / Q000378:metabolism / Q000652:urine*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D052616:Solid Phase Extraction / Q000379:methods*; D013237:Stereoisomerism; D014147:Tramadol / Q000031:analogs & derivatives* / Q000737:chemistry / Q000378:metabolism / Q000652:urine
chemical_list: D000701:Analgesics, Opioid; C080580:O-demethyltramadol; D014147:Tramadol