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

J Chromatogr B Analyt Technol Biomed Life Sci. 2019 Mar 1;1109:67-75. doi: 10.1016/j.jchromb.2019.01.020. Epub 2019 Jan 27.


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.

Keywords: 2-aminothiazoline-4-carboxylic acid; Cyanide biomarker; Magnetic carbon nanotubes facilitated dispersive micro solid phase extraction; Nanotechnology.

MeSH terms

  • Animals
  • Cattle
  • Cyanides / metabolism*
  • Gas Chromatography-Mass Spectrometry
  • Humans
  • Limit of Detection
  • Linear Models
  • Magnetite Nanoparticles / chemistry*
  • Nanotubes, Carbon / chemistry*
  • Reproducibility of Results
  • Solid Phase Extraction / methods*
  • Thiazoles / blood
  • Thiazoles / isolation & purification*
  • Thiazoles / metabolism
  • Thiazoles / urine


  • Cyanides
  • Magnetite Nanoparticles
  • Nanotubes, Carbon
  • Thiazoles
  • 2-amino-delta(2)-thiazoline-4-carboxylic acid