Determination of the cyanide metabolite 2-aminothiazoline-4-carboxylic acid in urine and plasma by gas chromatography-mass spectrometry.
The cyanide metabolite 2-aminothiazoline-4-carboxylic acid (ATCA) is a promising biomarker for cyanide exposure because of its stability and the limitations of direct determination of cyanide and more abundant cyanide metabolites. A simple, sensitive, and specific method based on derivatization and subsequent gas chromatography-mass spectrometry (GC-MS) analysis was developed for the identification and quantification of ATCA in synthetic urine and swine plasma. The urine and plasma samples were spiked with an internal standard (ATCA-d(2)), diluted, and acidified. The resulting solution was subjected to solid phase extraction on a mixed-mode cation exchange column. After elution and evaporation of the solvent, a silylating agent was used to derivatize the ATCA. Quantification of the derivatized ATCA was accomplished on a gas chromatograph with a mass selective detector. The current method produced a coefficient of variation of less than 6% (intra- and interassay) for two sets of quality control (QC) standards and a detection limit of 25 ng/ml. The applicability of the method was evaluated by determination of elevated levels of ATCA in human urine of smokers in relation to non-smokers for both males and females.
Logue
Brian A
BA
Department of Chemistry and Biochemistry, South Dakota State University, Shepard Hall 121, Box 2202, Brookings, SD 57007, USA. brian.logue@sdstate.edu
Kirschten
Nicholas P
NP
Petrikovics
Ilona
I
Moser
Matthew A
MA
Rockwood
Gary A
GA
Baskin
Steven I
SI
D000818:Animals; D002138:Calibration; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013552:Swine; D013844:Thiazoles / Q000032:analysis* / Q000097:blood / Q000652:urine
D013844:Thiazoles; C015674:2-amino-delta(2)-thiazoline-4-carboxylic acid