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An improved method for cyanide determination in blood using solid-phase microextraction and gas chromatography/mass spectrometry.
Rapid Commun Mass Spectrom. 2006; 20(19):2932-8.RC

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-microm carboxen/polydimethylsiloxane SPME fiber, with D3-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 microg/mL); and the LOD and LOQ in water were 0.006 and 0.01 microg/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.

Authors+Show Affiliations

Frison G
Forensic Toxicology and Antidoping, University Hospital of Padova, Via Falloppio 50, I-35121 Padova, Italy.
Zancanaro F
No affiliation info available
Favretto D
No affiliation info available
Ferrara SD
No affiliation info available

MeSH

CyanidesGas Chromatography-Mass SpectrometryHumansMicrochemistryReproducibility of ResultsSolid Phase ExtractionSpectrometry, Mass, Electrospray Ionization

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

16941546

Citation

Frison, Giampietro, et al. "An Improved Method for Cyanide Determination in Blood Using Solid-phase Microextraction and Gas Chromatography/mass Spectrometry." Rapid Communications in Mass Spectrometry : RCM, vol. 20, no. 19, 2006, pp. 2932-8.
Frison G, Zancanaro F, Favretto D, et al. An improved method for cyanide determination in blood using solid-phase microextraction and gas chromatography/mass spectrometry. Rapid Commun Mass Spectrom. 2006;20(19):2932-8.
Frison, G., Zancanaro, F., Favretto, D., & Ferrara, S. D. (2006). An improved method for cyanide determination in blood using solid-phase microextraction and gas chromatography/mass spectrometry. Rapid Communications in Mass Spectrometry : RCM, 20(19), 2932-8.
Frison G, et al. An Improved Method for Cyanide Determination in Blood Using Solid-phase Microextraction and Gas Chromatography/mass Spectrometry. Rapid Commun Mass Spectrom. 2006;20(19):2932-8. PubMed PMID: 16941546.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - An improved method for cyanide determination in blood using solid-phase microextraction and gas chromatography/mass spectrometry. AU - Frison,Giampietro, AU - Zancanaro,Flavio, AU - Favretto,Donata, AU - Ferrara,Santo Davide, PY - 2006/8/31/pubmed PY - 2007/9/7/medline PY - 2006/8/31/entrez SP - 2932 EP - 8 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun Mass Spectrom VL - 20 IS - 19 N2 - 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-microm carboxen/polydimethylsiloxane SPME fiber, with D3-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 microg/mL); and the LOD and LOQ in water were 0.006 and 0.01 microg/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. SN - 0951-4198 UR - https://www.unboundmedicine.com/medline/citation/16941546/An_improved_method_for_cyanide_determination_in_blood_using_solid_phase_microextraction_and_gas_chromatography/mass_spectrometry_ L2 - https://doi.org/10.1002/rcm.2689 DB - PRIME DP - Unbound Medicine ER -
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