Theoretical and experimental approach to hydrophilic interaction dispersive solid-phase extraction of 2-aminothiazoline-4-carboxylic acid from human post-mortem blood

J Chromatogr A. 2019 Feb 22:1587:61-72. doi: 10.1016/j.chroma.2018.12.028. Epub 2018 Dec 14.

Abstract

In this paper, we proposed an innovative hydrophilic interaction dispersive solid-phase extraction (HI-d-SPE) protocol suitable for the isolation of the potential cyanide intoxication marker, 2-aminothiazoline-4-carboxylic acid (ATCA), from such complicated matrix as post-mortem blood. To create an optimal HI-d-SPE protocol, two sorbents were used: a molecularly imprinted polymer (MIP) and commercially available Oasis-MCX®. The latter sorbent was identified as more recovery-efficient with higher clean-up abilities in a carefully optimized process. Computational analysis was employed to provide insight into the adsorption mechanism of the two selected sorbents. The theoretical results were in agreement with the experiment regarding the efficiency of the sorbent. HI-d-SPE was successfully applied to the analysis of ATCA in 20 post-mortem blood samples using LC-MS/MS. The analytical performance of the method was finally compared to prior existing methods, in turn revealing its superiority.

Keywords: 2-Aminothiazoline-4-carboxylic acid; Dispersive solid phase extraction; Human post-mortem blood; Mixed-mode cation exchange sorbent; Molecular modeling; Molecularly imprinted polymer.

MeSH terms

  • Adsorption
  • Biomarkers / blood*
  • Chromatography, Liquid
  • Diagnostic Techniques and Procedures*
  • Humans
  • Hydrophobic and Hydrophilic Interactions
  • Polymers
  • Reproducibility of Results
  • Solid Phase Extraction / methods*
  • Tandem Mass Spectrometry
  • Thiazoles / blood*
  • Thiazoles / isolation & purification*

Substances

  • Biomarkers
  • Polymers
  • Thiazoles
  • 2-amino-delta(2)-thiazoline-4-carboxylic acid