Solid-phase extraction and gas chromatographic- mass spectrometric determination of the veterinary drug xylazine in human blood.
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 microg/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.
Barroso
M
M
Instituto Nacional de Medicina Legal, Delegação de Coimbra, Largo da Sé Nova, 3000-213 Coimbra, Portugal. mjbarroso@iol.pt
Gallardo
E
E
Margalho
C
C
Devesa
N
N
Pimentel
J
J
Vieira
D N
DN
D000328:Adult; D004355:Drug Stability; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D008297:Male; D015203:Reproducibility of Results; D052616:Solid Phase Extraction; D014116:Toxicology / Q000379:methods*; D019155:Veterinary Drugs / Q000097:blood* / Q000737:chemistry / Q000633:toxicity; D014991:Xylazine / Q000097:blood* / Q000737:chemistry / Q000633:toxicity
D019155:Veterinary Drugs; D014991:Xylazine