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Simultaneous determination of cyanide and thiocyanate in plasma by chemical ionization gas chromatography mass-spectrometry (CI-GC-MS)

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Abstract

An analytical method utilizing chemical ionization gas chromatography-mass spectrometry was developed for the simultaneous determination of cyanide and thiocyanate in plasma. Sample preparation for this analysis required essentially one-step by combining the reaction of cyanide and thiocyanate with pentafluorobenzyl bromide and simultaneous extraction of the product into ethyl acetate facilitated by a phase-transfer catalyst, tetrabutylammonium sulfate. The limits of detection for cyanide and thiocyanate were 1 μM and 50 nM, respectively. The linear dynamic range was from 10 μM to 20 mM for cyanide and from 500 nM to 200 μM for thiocyanate with correlation coefficients higher than 0.999 for both cyanide and thiocyanate. The precision, as measured by %RSD, was below 9 %, and the accuracy was within 15 % of the nominal concentration for all quality control standards analyzed. The gross recoveries of cyanide and thiocyanate from plasma were over 90 %. Using this method, the toxicokinetic behavior of cyanide and thiocyanate in swine plasma was assessed following cyanide exposure.

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Acknowledgments

The research was supported by the CounterACT Program, National Institutes of Health Office of the Director, and the National Institute of Allergy and Infectious Diseases, Inter Agency Agreement Number Y1-OD-0690-01/A-120-B.P2010-01, Y1-OD-1561-01/A120-B.P2011-01, and the USAMRICD under the auspices of the US Army Research Office of Scientific Services Program Contract No. W911NF-11-D-0001 administered by Battelle (delivery order 0079, contract no TCN 11077). We gratefully acknowledge the funding from the Oak Ridge Institute for Science and Education (ORISE). The authors would also like to acknowledge Dr. George Perry, Associate Professor, Animal and Range Science of South Dakota State University, for making arrangements to provide swine plasma. The authors are thankful to Susan M. Boudreau, RN, BSN, Maria G. Castaneda, MS, Toni E. Vargas, PA-C, MHS, and Patricia Dixon, MHS, from the Clinical Research Division, Wilford Medical Center, Lackland A F B, TX, for providing cyanide exposed swine plasma samples for these studies. The opinions or assertions contained herein are the private views of the authors and are not to be construed as official or as reflecting the views of the Department of the Army, the National Institutes of Health, or the Department of Defense.

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Authors and Affiliations

  1. Department of Chemistry and Biochemistry, South Dakota State University, Avera Health and Science Center 131, Box 2202, Brookings, SD, 57007, USA

    Raj K. Bhandari, Robert P. Oda, Stephanie L. Youso & Brian A. Logue

  2. Department of Chemistry, Sam Houston State University, P.O. Box 2117, Huntsville, TX, 77341, USA

    Ilona Petrikovics

  3. Medical Toxicology, San Antonio Military Medical Center, United States Air Force, San Antonio, TX, 78229, USA

    Vikhyat S. Bebarta

  4. Analytical Toxicology Division, US Army Medical Research Institute of Chemical Defense, 3100 Ricketts Point Road, Aberdeen Proving Ground, MD, 21010-5400, USA

    Gary A. Rockwood

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  1. Raj K. Bhandari
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  7. Brian A. Logue
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Correspondence to Brian A. Logue.

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Bhandari, R.K., Oda, R.P., Youso, S.L. et al. Simultaneous determination of cyanide and thiocyanate in plasma by chemical ionization gas chromatography mass-spectrometry (CI-GC-MS). Anal Bioanal Chem 404, 2287–2294 (2012). https://doi.org/10.1007/s00216-012-6360-5

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