Journal Article

Chiral Analysis of Methadone and its Main Metabolite, EDDP, in Postmortem Brain and Blood by Automated SPE and Liquid Chromatography–Mass Spectrometry

Karen Marie Dollerup Holm and Kristian Linnet

in Journal of Analytical Toxicology

Volume 36, issue 7, pages 487-496
Published in print September 2012 | ISSN: 0146-4760
Published online July 2012 | e-ISSN: 1945-2403 | DOI: http://dx.doi.org/10.1093/jat/bks057
Chiral Analysis of Methadone and its Main Metabolite, EDDP, in Postmortem Brain and Blood by Automated SPE and Liquid Chromatography–Mass Spectrometry

More Like This

Show all results sharing these subjects:

  • Medical Toxicology
  • Toxicology (Non-medical)

GO

Show Summary Details

Preview

We developed a method based on liquid chromatography coupled with tandem mass spectrometry to quantify individual enantiomers of methadone and its primary metabolite, R/S-2-ethyl-1,5-dimethyl-3,3-diphenylpyrrolinium (EDDP), in postmortem blood and brain tissue. Samples were prepared with a Tecan Evo robotic system. Precipitation was followed by solid-phase extraction, evaporation and reconstitution in the mobile phase. Enantiomers were fully separated with liquid chromatography on a chiral α(1)-acid glycoprotein column. A Quattro micro mass spectrometer was used for detection in the positive ion mode with an electrospray source. The lower limit of quantification in brain tissue was 0.005 mg/kg for methadone and 0.001 mg/kg for EDDP enantiomers; the maximum precision was 17% for both compounds; accuracy ranged from 94 to 101%. In blood, the limit of quantification was 0.001 mg/kg for all compounds, the total relative standard deviation was <15%, and the accuracy varied from 95 to 109%. Brain (n = 11) and blood (n = 15) samples were analyzed with intermediate precision that varied from 7.5 to 15% at 0.005 mg/kg and from 6.8 to 11.3% at 0.25 mg/kg for all compounds. Method development focused on producing a clean extract, particularly from brain samples. The method was tested on authentic brain and femoral blood samples.

Journal Article.  6605 words.  Illustrated.

Subjects: Medical Toxicology ; Toxicology (Non-medical)

Full text: subscription required

How to subscribe Recommend to my Librarian

Users without a subscription are not able to see the full content. Please, subscribe or login to access all content.