Enatiomeric determination of tramadol and @@iO@-desmethyltramadol in human urine by gas chromatography- mass spectrometry

• Published in: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Analytical technologies in the biomedical and life sciences, 2009-07, Vol.877 (20-21), p.1937-1942
• Main Authors: Chytil, Lukas, Sticha, Martin, Matouskova, Olga, Perlik, Frantisek, Slanar, Ondrej
• Format: Article
• Language: English
• ISSN: 1570-0232
• DOI: 10.1016/j.jchromb.2009.04.042

A GC-MS assay for stereoselective determination of tramadol and its pharmacologically active phase I metabolite @@iO@-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 @@im@/@@iz@ 263; 58, 249; 58, and 179; 58 for the determination of concentration of tramadol, @@iO@-desmethyltramadol and internal standard, respectively. Chromatography was performed on a Rt-bDEXcst column containing alkylated beta-cyclodextrins as a chiral selector. The calibration curves were linear in the concentration range 0.1-20 kg/mL (@@iR@@@u2@ > = 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.