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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 26, Number 3, April,
pp. 144-148
Determination of Blood Cyanide by HPLC–MS
A. Tracqui, J.S. Raul, A. Géraut, L. Berthelon,
and B. Ludes
Institut de Médecine Légale, 11 rue Humann, 67085 Strasbourg,
France
An original high-performance
liquid chromatographic–mass spectrometric (HPLC–MS) procedure was
developed for the determination of cyanide (CN) in whole blood. After the addition
of K13C15N as internal standard, blood was placed in a microdiffusion device,
the inner well of which was filled with a mixture of taurine (50mM in water)/naphthalene-2,3-dicarboxaldehyde
(NDA, 10mM in methanol)/methanol/ concentrated (approximately 20%) ammonia solution
(25:25:45:5, v/v). Concentrated H2SO4 was added to the blood sample, and the
microdiffusion chamber was sealed. After 30 min of gentle agitation, 2 µL
of the contents of the inner vial were pipetted and directly injected onto a
NovaPak C18 HPLC column. Separation was performed by a gradient of acetonitrile
in 2mM NH4COOH, pH 3.0 buffer (35–80% in 10 min). Detection was done with
a Perkin-Elmer Sciex API-100 mass analyzer with an ionspray interface, operated
in the negative ionization mode. MS data were collected as either TIC or SIM
at m/z (299 + 191) and (301 + 193) for the derivatives formed with CN and 13C15N,
respectively. Inspired by previous works dealing with the complexation of CN
by NDA + taurine to form a 1-cyano [f] benzoisoindole derivative analyzed by
HPLC–fluorimetry, this method appears simple, rapid, and extremely specific.
Limits of detection and quantitation for blood CN are 5 and 15 ng/mL, respectively.
The use of 13C15N as internal standard allows the quantitation of CN with elegance
and accuracy in comparison with previously reported methods. Reproduction
of editorial content of this journal is prohibited without publisher’s
permission.
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