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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 26, Number 6, September 2002,
pp. 320-324
Simultaneous Determination of Nitrate and Nitrite in Human
Plasma by Gas Chromatography–Mass Spectrometry
Shigetoshi Kage[1], Keiko Kudo[2], and Noriaki Ikeda[2]
[1]Forensic Science Laboratory, Fukuoka Prefectural Police Headquarters, 7-7,
Higashikoen, Hakata-ku, Fukuoka 812-8576, Japan and
[2]Department of Forensic Pathology and Sciences, Graduate School of Medical
Sciences, Kyushu University, 3-1-1, Maidashi, Higashi-ku, Fukuoka 812-8582,
Japan
We devised a sensitive and
simple method for the simultaneous determination of nitrate and nitrite in human
plasma, using extractive alkylation. These inorganic anions were alkylated with
pentafluorobenzyl bromide, using tetradecyldimethylbenzylammonium chloride as
the phase-transfer catalyst, with 1,3,5-tribromobenzene as an internal standard.
The derivatives were analyzed by gas chromatography–mass spectrometry,
using the negative-ion chemical ionization mode with isobutane as the reagent
gas. Calibration curves for nitrate and nitrite were linear over the concentration
range of 0.01 to 1.0 µmol/mL in plasma, and the lower limit of detection
for both compounds was 0.005 µmol/mL. The accuracy and precision of this
method were evaluated and coefficients of variation were lower than 10.4%. Blood
nitrate and nitrite concentrations of six victims who committed suicide by inhaling
automobile exhaust gas could be determined using our method. Reproduction
of editorial content of this journal is prohibited without publisher’s
permission.
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