A selective adsorption-based separation of low-mass molecules from biological samples towards high-throughput mass spectrometry analysis in a single drop of human whole blood

Talanta. 2019 Sep 1:202:237-243. doi: 10.1016/j.talanta.2019.05.005. Epub 2019 May 4.

Abstract

In this work, a newly designed multifunctional adsorbent material, octadecyl-modified ordered mesoporous carbon (C18-CMK-8), was synthesized and employed for simultaneous analysis of multiple small molecules by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS). The C18-CMK-8 was facilely prepared by one-step chemical binding of octadecyltrimethoxysilane to an ordered mesoporous carbon CMK-8. The nanosized pore structure of C18-CMK-8 can selectively enrich low-mass molecules while excluding interferences from large molecules in whole blood; meanwhile, the C18 chain can greatly enhance the affinity for a wide range of small molecules. Then, the C18-CMK-8-based solid-phase extraction (SPE) combined with MALDI-TOF MS measurement was applied in rapid and high-throughput screening of six doping agents (triamterene, trenbolone, testosterone, methyltestosterone, clenbuterol, and strychnine)) in single-drop human whole blood samples. The method showed high analytical sensitivity (detection limit 0.05-0.1 ng mL-1), good recoveries (67.2-114.3%), minimal sample requirement (∼20 μL), and robust anti-interference ability. With distinct advantages such as high throughput, rapidness, minimal sample requirement, and high sensitivity, this study not only offers a versatile enrichment material for complex sample preparation, but also demonstrates a promising tool for minimal whole blood analysis.

Keywords: Adsorbent; MALDI-TOF MS; Mass spectrometry; Ordered mesoporous carbon; Sample preparation; Single-drop whole blood.

MeSH terms

  • Adsorption
  • Blood Chemical Analysis*
  • Carbon / blood*
  • Humans
  • Mass Spectrometry
  • Molecular Weight
  • Particle Size
  • Porosity
  • Silanes / blood*
  • Surface Properties

Substances

  • Silanes
  • Carbon
  • trimethoxysilane