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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 31, Number 3, April 2007,
pp.165-169
TECHNICAL NOTE: Solid-Phase Extraction and Gas Chromatographic–
Mass Spectrometric Determination of the Veterinary Drug Xylazine in Human Blood
M. Barroso[1], E. Gallardo[2], C. Margalho[1], N. Devesa[3],
J. Pimentel[3], and D.N. Vieira[1]
[1]Instituto Nacional de Medicina Legal, Delegação de Coimbra,
Largo da Sé Nova, 3000-213 Coimbra, Portugal;
[2]Instituto de Medicina Legal, Servicio de Toxicología Forense, Universidad
de Santiago de Compostela, San Francisco s/n, 15782 Santiago de Compostela,
Spain; and
[3]Serviço de Medicina Interna, Hospitais da Universidade de Coimbra,
Praceta Mota Pinto, 3000-075 Coimbra, Portugal
This paper presents a method for the determination of xylazine
in whole blood using solid-phase extraction and gas chromatography–mass
spectrometry. This technique required only 0.5 mL of sample, and protriptyline
was used as internal standard (IS). Limits of detection and quantitation (LOQ)
were 2 and 10 ng/mL, respectively. The method was found to be linear between
the LOQ and 3.50 µg/mL, with correlation coefficients higher than 0.9922.
Precision (intra- and interday) and accuracy were in conformity with the criteria
normally accepted in bioanalytical method validation. The analyte was stable
in the matrix for at least 18 h at room temperature and for at least three freeze/thaw
cycles. Mean recovery, calculated at three concentration levels, was 87%. To
the best of our knowledge, this is the first time that solid-phase extraction
is used as sample preparation technique for the determination of this compound
in biological media. Because of its simplicity and speed when compared to other
extraction techniques, the herein described method can be successfully applied
in the diagnosis of intoxications by xylazine.
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