Gas chromatographic method for the sensitive determination of 2,5-hexanedione using electron capture and mass-selective detection (Journal article)

Konidari, C. N./ Stalikas, C. D./ Karayannis, M. I.


2,5-Hexanedione (2,5HD) is the principle metabolite of n-hexane and methyl ethyl ketone in human urine. In this paper, a rapid and highly sensitive method for the determination of urinary 2,5HD by gas chromatography-electron capture detection and gas chromatography-mass selective detection is described. The method comprises, optionally, acid hydrolysis before the analyte is being derivitized with 2,4,6-trichlorophenyl hydrazine (TCPH) towards the formation of a chlorinated hydrazone derivative for 2,5HD analysis. The reaction conditions such as temperature, time, reagent concentration and pH were optimized properly. The detection limit of the method - defined as signal to noise ratio = 3 - is as low as 0.4 and 1.5 muM using the ECD and MSD (SIM mode), respectively. The linearity of the detection systems extends up to 50 muM of 2,5HD with correlation coefficients better than 0.9995. The within-day and between-day reproducibility for a urine sample of 10 muM in 2,5HD were 2.6 and 3.2%, respectively. Spiked pooled samples with various concentrations in the range 5-10 muM were processed following the proposed procedure. The recovery was satisfactory enough ranging from 92 to 104%. The method was applied to the analysis of urine samples received from people working in a chemical laboratory and the results revealed variable, yet low concentrations of 2,5HD in the hydrolyzed samples. (C) 2001 Elsevier Science B.V. All rights reserved.
Institution and School/Department of submitter: Πανεπιστήμιο Ιωαννίνων. Σχολή Θετικών Επιστημών. Τμήμα Χημείας
Keywords: 2,5-hexanedione (2,5hd),2,4,6-trichlorophenyl hydrazine (tcph),gas chromatography,performance liquid-chromatography,n-hexane metabolites,ethyl-ketone mek,urinary 2,5-hexanedione,occupational exposure,derivatization,spectrometry,coexposure,protein
URI: http://olympias.lib.uoi.gr/jspui/handle/123456789/8034
ISSN: 0003-2670
Publisher: Elsevier
Item type: journalArticle
Link: <Go to ISI>://000170757300006
http://ac.els-cdn.com/S0003267001010820/1-s2.0-S0003267001010820-main.pdf?_tid=c3ff6b95410547102b00ebb17fec6cb2&acdnat=1333040857_507ce0391f7e11f53947c0006e1e181a
Item language: en
Item access scheme: campus
Institution and School/Department of submitter: Πανεπιστήμιο Ιωαννίνων. Σχολή Θετικών Επιστημών. Τμήμα Χημείας
Publication date: 2001
Abstract: 2,5-Hexanedione (2,5HD) is the principle metabolite of n-hexane and methyl ethyl ketone in human urine. In this paper, a rapid and highly sensitive method for the determination of urinary 2,5HD by gas chromatography-electron capture detection and gas chromatography-mass selective detection is described. The method comprises, optionally, acid hydrolysis before the analyte is being derivitized with 2,4,6-trichlorophenyl hydrazine (TCPH) towards the formation of a chlorinated hydrazone derivative for 2,5HD analysis. The reaction conditions such as temperature, time, reagent concentration and pH were optimized properly. The detection limit of the method - defined as signal to noise ratio = 3 - is as low as 0.4 and 1.5 muM using the ECD and MSD (SIM mode), respectively. The linearity of the detection systems extends up to 50 muM of 2,5HD with correlation coefficients better than 0.9995. The within-day and between-day reproducibility for a urine sample of 10 muM in 2,5HD were 2.6 and 3.2%, respectively. Spiked pooled samples with various concentrations in the range 5-10 muM were processed following the proposed procedure. The recovery was satisfactory enough ranging from 92 to 104%. The method was applied to the analysis of urine samples received from people working in a chemical laboratory and the results revealed variable, yet low concentrations of 2,5HD in the hydrolyzed samples. (C) 2001 Elsevier Science B.V. All rights reserved.
Publisher: Elsevier
Journal name: Analytica Chimica Acta
Journal type: peer reviewed
Appears in Collections:Άρθρα σε επιστημονικά περιοδικά ( Ανοικτά)

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