Journal
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
Volume 926, Issue -, Pages 9-15Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.jchromb.2013.02.019
Keywords
Tramadol; O-Desmethyltramadol; N-Desmethyltramadol; Urine; GC/MS; Validation
Funding
- Analytical Unit, St. George's - University of London
- Bo Holmstedt Memorial Foundation
- Southern and Eastern African Network for Analytical Chemists (SEANAC)
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Analytical procedures for the determination of tramadol (T), O-desmethyltramadol (ODT), and N-desmethyltramadol (NDT) in human urine have been developed and validated using gas chromatography-mass spectrometry (GC/MS). Sample preparation involved liquid-liquid extraction with methyl-tert-butyl ether (MTBE) and followed by back extraction with 0.1 M hydrochloric acid. Proadifen (SKF525A) was selected as internal standard (IS). Extraction efficiencies of T, ODT and NDT were 102.12, 101.30, and 98.21%, respectively. The calibration curves were linear (r(2) > 0.99) in the concentration range 10-1000 ng/mL for all compounds. Limits of quantification (LOQ) were 10,10 and 20 ng/mL for T, ODT and NDT, respectively. Intra-assay precision was within 1.29-6.48% and inter-assay precision was within 1.28-6.84% for T, ODT and NDT. Intra-assay accuracy was within 91.79-106.89% for all analytes. This method detected urine concentrations of T, ODT and NDT in six healthy volunteers for 7 days after administration of 50 mg oral doses of tramadol. (C) 2013 Elsevier B.V. All rights reserved.
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