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An improved method for cyanide determination in blood using solid‐phase microextraction and gas chromatography/mass spectrometry
Author(s) -
Frison Giampietro,
Zancanaro Flavio,
Favretto Donata,
Ferrara Santo Davide
Publication year - 2006
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.2689
Subject(s) - chemistry , solid phase microextraction , chromatography , detection limit , hydrogen cyanide , mass spectrometry , gas chromatography–mass spectrometry , aqueous solution , gas chromatography , selected ion monitoring , adsorption , cyanide , analytical chemistry (journal) , inorganic chemistry , organic chemistry
Abstract A new method is described for the qualitative and quantitative analysis of cyanide, a very short‐acting and powerful toxic agent, in human whole blood. It involves the conversion of cyanide into hydrogen cyanide and its subsequent headspace solid‐phase microextraction (HS‐SPME) and detection by gas chromatography/mass spectrometry (GC/MS) in selected ion monitoring (SIM) mode. Optimizing the conditions for the GC/MS (type of column, injection conditions, temperature program) and SPME (choice of SPME fiber, effect of salts, adsorption and desorption times, adsorption temperature) led to the choice of a 75‐µm carboxen/polydimethylsiloxane SPME fiber, with D 3 ‐acetonitrile as internal standard, and a capillary GC column with a polar stationary phase. Method validation was carried out in terms of linearity, precision and accuracy in both aqueous solutions and blood. The limit of detection (LOD) and limit of quantitation (LOQ) were determined only in aqueous solutions. The assay is linear over three orders of magnitude (water 0.01–10, blood 0.05–10 µg/mL); and the LOD and LOQ in water were 0.006 and 0.01 µg/mL, respectively. Good intra‐ and inter‐assay precision was obtained, always <8%. The method is simple, fast and sensitive enough for the rapid diagnosis of cyanide intoxication in clinical and forensic toxicology. Copyright © 2006 John Wiley & Sons, Ltd.