Determination of volatile substances in biological samples by headspace gas chromatography

Seto, Yasuo

doi:10.1016/0021-9673(94)85216-2

Cited by 91 publications

(84 citation statements)

References 257 publications

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“…Salt addition was studied to determine the salting out effect on analyte extraction, as indicated by some investigators who use headspace technique for several volatile chemicals extraction 26,27,29,30 . According to Seto 29 the solubility of many non-electrolyte compounds is reduced by salt addition due to an increase in the activity coefficient (y).…”

Section: Resultsmentioning

confidence: 99%

“…This technique is simple, requires little sample handling and eliminates non-volatile interferents that might contaminate the GC injector and FID detector. The critical point is the equilibrium between the condensed phase and the vapor phase [25][26][27][28][29] and several parameters must be optimized to guarantee maximum analyte recovery and sensitivity of the method. Since the determination of urinary acetone is of interest in various situations, the objective of the present study was to optimizing a rapid and low cost technique that could be applied in clinical and toxicological routine analysis in laboratories with limited resources, establishing the better conditions to extract AcU by static headspace and to quantify by GC/FID.…”

Section: Introductionmentioning

confidence: 99%

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A simple and rapid method for urinary acetone analysis by headspace/gas chromatography

Oliveira¹,

Siqueira²

2007

Quím. Nova

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Recebido em 31/5/06; aceito em 9/11/06; publicado na web em 6/8/07Urinalysis of acetone is important to monitor workers occupationally exposed to acetone and/or isopropanol, as well as in diagnosis of some diseases related to lipid metabolism impairment. This work shows a sensitive, simple and rapid static headspace-gas chromatographic procedure for quantitative determination of acetone in urine. The method was applied to measure acetone in 207 samples from general population volunteers, resulting in a mean level of 1.12 mg/L (± 0.47) and a range of 0.20 -1.95 mg/L. The method is reproducible and reliable, making it suitable for routine analysis of acetone in urine.

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

A simple and rapid method for urinary acetone analysis by headspace/gas chromatography

Oliveira¹,

Siqueira²

2007

Quím. Nova

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“…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

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-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. ...

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“…The technique of static headspace gas chromatography has great acceptance in the forensic field, especially for the determination of ethanol in biological samples (Macchia et al, 1995;Tagliaro et al, 1992), so most forensic laboratories in the world have this equipment and perform this analysis on a routine basis, but in many of these laboratories, equipment is exclusively employed to determine ethanol, even when this technique can be used to determine many other substances of toxicological interest, volatile substances, without major changes to the equipment (Seto, 1994), thus we can conclude that these laboratories do not exploit all the possibilities of the technique.…”

Section: Introductionmentioning

confidence: 99%

“…The determination of volatile substances in forensic samples has been carried out through titrations, spectrophotometric methods and chromatographic methods, as well (Seto, 1994). Titrations and spectrophotometric methods are not specific and usually lack sufficient sensitivity, besides not being able to analyze simultaneously all the volatile substances.…”

Section: Introductionmentioning

confidence: 99%

Determination of Volatile Substances in Forensic Samples by Static Headspace Gas Chromatography

Bernal¹

2012

Gas Chromatography in Plant Science, Wine Technology, Toxicology and Some Specific Applications

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Determination of volatile substances in biological samples by headspace gas chromatography

Cited by 91 publications

References 257 publications

A simple and rapid method for urinary acetone analysis by headspace/gas chromatography

A simple and rapid method for urinary acetone analysis by headspace/gas chromatography

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

Determination of Volatile Substances in Forensic Samples by Static Headspace Gas Chromatography

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