Determination of blood cyanide by headspace gas chromatography with nitrogen-phosphorus detection and using a megabore capillary column

Seto, Yasuo; Tsunoda, Noriko; Ohta, Hikoto; Shinohara, Toshiaki

doi:10.1016/0003-2670(93)80391-w

Cited by 65 publications

(52 citation statements)

References 38 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…According to the manufacturer's specifications the CP PoraBOND Q column is a bonded porous polymer PLOT column exhibiting low bleed and high stability under exposure to water. A similar type of stationary phase, in combination with an FTD, was previously employed for separation and detection of cyanides from the headspace of blood samples (Seto et al, 1993).…”

Section: Configurationmentioning

confidence: 99%

A gas chromatographic instrument for measurement of hydrogen cyanide in the lower atmosphere

et al. 2012

View full text Add to dashboard Cite

Abstract. A gas-chromatographic (GC) instrument was developed for measuring hydrogen cyanide (HCN) in the lower atmosphere. The main features of the instrument are (1) a cryogen-free cooler for sample dehumidification and enrichment, (2) a porous polymer PLOT column for analyte separation, (3) a flame thermionic detector (FTD) for sensitive and selective detection, and (4) a dynamic dilution system for calibration. We deployed the instrument for a ∼4 month period from January-June, 2010 at the AIRMAP atmospheric monitoring station Thompson Farm 2 (THF2) in rural Durham, NH. A subset of measurements made during 3-31 March is presented here with a detailed description of the instrument features and performance characteristics. The temporal resolution of the measurements was ∼20 min, with a 75 s sample capture time. The 1σ measurement precision was <10 % and the instrument response linearity was excellent on a calibration scale of 0.10-0.75 ppbv (±5 %). The estimated method detection limit (MDL) and accuracy were 0.021 ppbv and 15 %, respectively. From 3-31 March 2010, ambient HCN mixing ratios ranged from 0.15-1.0 ppbv (±15 %), with a mean value of 0.36 ± 0.16 ppbv (1σ ). The approximate mean background HCN mixing ratio of 0.20 ± 0.04 ppbv appeared to agree well with tropospheric column measurements reported previously. The GC-FTD HCN measurements were strongly correlated with acetonitrile (CH 3 CN) measured concurrently with a proton transfer-reaction mass spectrometer (PTR-MS), as anticipated given our understanding that the nitriles share a common primary biomass burning source to the global atmosphere. The nitriles were overall only weakly correlated with carbon monoxide (CO), which is reasonable considering the greater diversity of sources for CO. However, strong correlations with CO were observed on several nights under stable atmospheric conditions and suggest regional combustion-based sources for the nitriles. These results demonstrate that the GC-FTD instrument is capable of making long term, in-situ measurements of HCN in the lower atmosphere. To date, similar measurements have not been performed, yet they are critically needed to (1) better evaluate the regional scale distribution of HCN in the atmosphere and (2) discern the influence of biomass burning on surface air composition in remote regions.

show abstract

Section: Configurationmentioning

confidence: 99%

A gas chromatographic instrument for measurement of hydrogen cyanide in the lower atmosphere

et al. 2012

View full text Add to dashboard Cite

show abstract

“…The evolved HCN is either absorbed in a basic solution or sampled directly from the headspace before detection. Detection has been based on colorimetry (8 ), fluorometry (2,9 ), HPLC-mass spectrometry (MS) (10 ), and gas chromatography (GC) with electron capture (11,12 ), nitrogen-phosphorus (5,(13)(14)(15), and MS detection (16,17 ). The determination of CN by equilibrium headspace analysis appears most efficient, with analysis times ranging from 17 to 40 min per sample; however, accurate analysis depends on a matched, interference-free response between CN and an internal standard.…”

mentioning

confidence: 99%

Determination of Cyanide in Blood by Isotope-Dilution Gas Chromatography–Mass Spectrometry

Murphy¹,

Schantz²,

Butler³

et al. 2006

Clinical Chemistry

View full text Add to dashboard Cite

Background: Cyanide (CN) is a lethal toxin. Quantification in blood is necessary to indicate exposure from many sources, including food, combustion byproducts, and terrorist activity. We describe an automated procedure based on isotope-dilution gas chromatographymass spectrometry (ID GC/MS) for the accurate and rapid determination of CN in whole blood. Methods: A known amount of isotopically labeled potassium cyanide (K 13 C 15 N) was added to 0.5 g of whole blood in a headspace vial. Hydrogen cyanide was generated through the addition of phosphoric acid, and after a 5-min incubation, 0.5 mL of the headspace was injected into the GC/MS at an oven temperature of

show abstract

“…Hydrogen cyanide was detected at 2.2 min. This method provides very sensitive determination of cyanide (limit of detection: about 0.5 ng/mL, S /N = 3) with a wide range linearity [15]. From the background nitrite solution (50 mM), the unknown peak was eluted just at the same position of hydrogen cyanide.…”

Section: Resultsmentioning

confidence: 99%

“…Produced cyanide was quantified by HS-GC [14] under the following analytical conditions [15]. Gas chromatograph, HP6890 (Agilent Technologies, Tokyo, Japan) was used with a porous polymer capillary column of GS-Q (30 m × 0.53 mm i.d., J&W Scientific, Folson, CA, USA) and a nitrogen-phosphorus detector maintained at 250 • C. Column temperature was set at 140 • C. Flow rate of the carrier gas (helium) was 5 mL/min.…”

Section: Incubation Of Samples With Nitrite and Determination Of Cyanmentioning

confidence: 99%

Artifactual production of cyanide from coffee and tea drinks in the presence of nitrite

et al. 2008

Self Cite

View full text Add to dashboard Cite

-Introduction:In cases of unknown poisoning, forensic toxicologists are required to elucidate the cause of death, and one of the most noticeable poisons is cyanide. We report on the artifactual production of cyanide from coffee and tea drinks in the presence of nitrite, which is frequently adulterated to lead to the fault result in drug testing. Methods: Cyanide was measured by head-space gas chromatography using porous polymer capillary GS-Q column and a nitrogen-phosphorus detector. Samples were mixed with sodium nitrite in a glass vial under acidic conditions of 10% phosphoric acid or 0.6 M sodium phosphate buffer (pH 5.0). After incubation for 30 min at 50 • C, the resulting head-space was injected into the gas chromatograph. Hydrogen cyanide was eluted at 2.2 min, and the peak area was converted for measuring cyanide concentration in the liquid reaction mixture. From the 50 • C incubation mixture of commercial coffee drink (or tea drink) and nitrite (50 mM), several µg/mL and sub-µg/mL of cyanide was produced in the presence of 10% phosphoric acid and pH 5.0 buffer, respectively. Cyanide was also produced from the reaction mixture of nitrite and polyphenol compounds such as chlorogenic acid and catechins, which are included in coffee and tea drinks, but not from a monophenol mixture. The amount of cyanide produced was dependent on substrate concentrations of nitrite and polyphenol, pH, temperature and incubation time. Conclusion: Forensic toxicologists should pay attention to this type of artifactual production of cyanide.Key words: Cyanide, false positive detection, polyphenol, nitrite Résumé -Introduction : Dans les cas d'empoisonnement mystérieux, il est demandé aux médecins légistes de déter-miner la cause du décès, et notamment la présence de cyanure. Nous avons examiné la production faussement positive de cyanure à partir de thé et de café en présence de nitrites, fréquemment employés pour fausser les tests de détection. Méthodes : La teneur en cyanure a été établie par chromatographie gazeuse d'espace de tête avec une colonne capillaire GS-Q sur polymère poreux et un détecteur azote-phosphore. Les échantillons ont été mélangés à du nitrite de sodium dans une fiole en verre, en acidifiant par 10 % d'acide phosphorique ou par un tampon de phosphate de sodium 0,6 M (pH 5,0). Après incubation à 50 • C pendant 30 min, l'espace de tête résultant était injecté dans le chromatographe. Le cyanure d'hydrogène est élué en 2,2 min, et l'espace de tête a été traité pour mesurer la concentration en cyanure dans le mélange liquide siège de la réaction. Dans le mélange café (ou thé) vendu dans le commerce et nitrite (50 mM) ayant incubé à 50 • C, moins de 1 µg/mL et plusieurs µg/mL de cyanure ont été produits en présence, respectivement, de 10 % d'acide phosphorique et du tampon à pH 5,0. Le cyanure a aussi pu être produit par réaction au mélange avec des nitrites ou des polyphénols tels que l'acide chlorogénique et les catéchines, qui sont contenus dans le thé et le café, mais pas à partir de monophénols. ...

show abstract

Determination of blood cyanide by headspace gas chromatography with nitrogen-phosphorus detection and using a megabore capillary column

Cited by 65 publications

References 38 publications

A gas chromatographic instrument for measurement of hydrogen cyanide in the lower atmosphere

A gas chromatographic instrument for measurement of hydrogen cyanide in the lower atmosphere

Determination of Cyanide in Blood by Isotope-Dilution Gas Chromatography–Mass Spectrometry

Artifactual production of cyanide from coffee and tea drinks in the presence of nitrite

Contact Info

Product

Resources

About