Journal Article

Simultaneous Identification of the Enantiomers and Diastereomers of <i>N</i>,<i>O</i>-Di-trifluoroacetylated Ephedrine and Norephedrine in Blood Plasma using Chiral Capillary Gas Chromatography–Mass Spectrometry with Selected Ion Monitoring

Toshiaki Nagai, Akira Kurosu, Kazumi Matsushima, Junko Maeda, Atsushi Tohei, Shinobu Yamauchi, Masahito Hitosugi and Shogo Tokudome

in Journal of Analytical Toxicology

Volume 36, issue 2, pages 96-105
Published in print March 2012 | ISSN: 0146-4760
Published online March 2012 | e-ISSN: 1945-2403 | DOI: http://dx.doi.org/10.1093/jat/bkr010
Simultaneous Identification of the Enantiomers and Diastereomers of N,O-Di-trifluoroacetylated Ephedrine and Norephedrine in Blood Plasma using Chiral Capillary Gas Chromatography–Mass Spectrometry with Selected Ion Monitoring

More Like This

Show all results sharing these subjects:

  • Medical Toxicology
  • Toxicology (Non-medical)

GO

Show Summary Details

Preview

A method for identifying the enantiomers of N,O-di-trifluoroacetylated ephedrine (EP) and norephedrine (NE) and the enantiomers of pseudoephedrine (PEP) and pseudonorephedrine (PNE) in plasma was developed using chiral capillary gas chromatography–mass spectrometry (GC–MS) with selected ion monitoring (SIM). N,O-Di-trifluoroacethyl (TFA) derivatization was accomplished in a dried hydrochloride extract of plasma (minimum quantity of 0.2 mL). An SIM GC–MS method with a β-cyclodextrin chiral capillary column allowed the successful and simultaneous detection of each TFA-derivatized stereoisomer of EP, NE, PEP, PNE, and an internal standard (IS; S-(+)-ethylamphetamine). Each TFA-drivatized stereoisomer was identified using four mass fragment ions (m/z 140, 154, 168, and 230). The TFA-derivatized stereoisomers of EP, NE, PEP, PNE, and IS were separated completely and were detected with sufficient sensitivity. The assay allowed the stereoisomers to be determined in a linear range of 12.5–1250 ng/mL for the EP stereoisomers and a linear range of 5–1250 ng/mL for the PEP, NE, and PNE stereoisomers. The detection limits were 7.5 ng/mL for the EP stereoisomers and 2.5 ng/mL for the PEP, NE, and PNE stereoisomers. The intra- and interday precisions were less than 5.9% and 8.2%, respectively. This chiral capillary SIM GC–MS method was sufficiently effective in the analysis of plasma from users of over-the-counter cold medicines and was also fully applicable to the plasma analysis of guinea pigs following their treatment with racemic EP.

Journal Article.  5620 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.