Original Paper

Analytical and Bioanalytical Chemistry

, Volume 404, Issue 8, pp 2287-2294

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

  • Raj K. BhandariAffiliated withDepartment of Chemistry and Biochemistry, South Dakota State University
  • , Robert P. OdaAffiliated withDepartment of Chemistry and Biochemistry, South Dakota State University
  • , Stephanie L. YousoAffiliated withDepartment of Chemistry and Biochemistry, South Dakota State University
  • , Ilona PetrikovicsAffiliated withDepartment of Chemistry, Sam Houston State University
  • , Vikhyat S. BebartaAffiliated withMedical Toxicology, San Antonio Military Medical Center, United States Air Force
  • , Gary A. RockwoodAffiliated withAnalytical Toxicology Division, US Army Medical Research Institute of Chemical Defense
  • , Brian A. LogueAffiliated withDepartment of Chemistry and Biochemistry, South Dakota State University Email author 

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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.

Keywords

Cyanide Thiocyanate Method development Chemical-ionization gas-chromatography mass-spectrometry