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LC-MS/MS Method for the determination of carbamathione in human plasma
Heemskerk, Anthonius A. M. Haandel, Leon van Wood, Joshua M. McCance-Katz, Elinore F. Williams, Todd D. Stobaugh, John F. Faiman, Morris D.
Heemskerk, Anthonius A. M.
Haandel, Leon van
Wood, Joshua M.
McCance-Katz, Elinore F.
Williams, Todd D.
Stobaugh, John F.
Faiman, Morris D.
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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 ∼98%). 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 8 minutes. Calibration was established and validated over the concentration range of 0.5-50 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 (250 mg/d). Interestingly, an unknown but apparently related metabolite was observed with each human plasma sample analyzed.
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Date
2011-03-25
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Elsevier
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Keywords
LC-MS/MS, Carbamathione, Disulfuram, Glutathione conjugates
Citation
Heemskerk, A. A. M., van Haandel, L., Woods, J. M., McCance-Katz, E. F., Williams, T. D., Stobaugh, J. F., & Faiman, M. D. (2011). LC-MS/MS Method for the determination of carbamathione in human plasma. Journal of Pharmaceutical and Biomedical Analysis, 54(4), 799–806. http://doi.org/10.1016/j.jpba.2010.10.021