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Development of magnetic carbon nanotubes for dispersive micro solid phase extraction of the cyanide metabolite, 2-aminothiazoline-4-carboxylic acid, in biological samples

Li, Sun Yi, Petrikovics, Ilona, Yu, Jorn (Chi Chung)
Journal of chromatography 2019 v.1109 pp. 67-75
biomarkers, blood, carbon, carbon nanotubes, carboxylic acids, cattle, cyanides, gas chromatography-mass spectrometry, magnetism, metabolism, metabolites, solid phase extraction, sorbents, stable isotopes, urine
2-aminothiazoline-4-carboxylic acid (ATCA) is a minor metabolite of cyanide and is suggested to be a promising biomarker for cyanide exposure due to its specificity to cyanide metabolism and its excellent short- and long-term stability during storage. In this study, magnetic carbon nanotubes, including magnetic multi-walled carbon nanotubes (Mag-MWCNT) and magnetic single-walled carbon nanotubes (Mag-SWCNT) were synthesized as a novel sorbent for dispersive micro solid phase extraction (d-μSPE) to extract ATCA from biological matrices. ATCA spiked deionized water samples with the addition of the isotopic internal standard (ATCA – 13C, 15N) were subjected to Mag-CNT/d-μSPE to confirm extraction efficiency of this new technique. The extracted ATCA was derivatized and quantitated using gas chromatography/mass spectrometry (GC/MS) analysis. The extraction parameters were optimized and a detection limits of 15 and 25 ng/mL were obtained for synthetic urine and bovine blood respectively with a linear dynamic range of 30–1000 ng/mL. The optimized Mag-CNT/d-μSPE method facilitated efficient extraction of ATCA using 2 mg of Mag-MWCNT with a 10-minute extraction time. The current assay was also found to be effective for the extraction of ATCA with average recoveries of 97.7 ± 4.0% (n = 9) and 96.5 ± 12.1% (n = 9) from synthetic urine and bovine blood respectively. The approach of using Mag-CNT to facilitate d-μSPE offered a novel alternative to extract ATCA from complex biological matrices.