Article ID | Journal | Published Year | Pages | File Type |
---|---|---|---|---|
10553552 | Journal of Pharmaceutical and Biomedical Analysis | 2011 | 8 Pages |
Abstract
Liquid chromatography-tandem mass spectrometry methodology is described for the determination of S-(N,N-diethylcarbamoyl)glutathione (carbamathione) in human plasma samples. Sample preparation consisted of a straightforward perchloric acid medicated protein precipitation, with the resulting supernatant containing the carbamathione (recovery â¼98%). For optimized chromatography/mass spec detection a carbamathione analog, S-(N,N-di-i-propylcarbamoyl)glutathione, was synthesized and used as the internal standard. Carbamathione was found to be stable over the pH 1-8 region over the timeframe necessary for the various operations of the analytical method. Separation was accomplished via reversed-phase gradient elution chromatography with analyte elution and re-equilibration accomplished within 8Â min. Calibration was established and validated over the concentration range of 0.5-50Â nM, which is adequate to support clinical investigations. Intra- and inter-day accuracy and precision determined and found to be <4% and <10%, respectively. The methodology was utilized to demonstrate the carbamathione plasma-time profile of a human volunteer dosed with disulfiram (250Â mg/d). Interestingly, an unknown but apparently related metabolite was observed with each human plasma sample analyzed.
Keywords
Related Topics
Physical Sciences and Engineering
Chemistry
Analytical Chemistry
Authors
Anthonius A.M. Heemskerk, Leon van Haandel, Joshua M. Woods, Elinore F. McCance-Katz, Todd D. Williams, John F. Stobaugh, Morris D. Faiman,