A sediment extraction and cleanup method for wide-scope multitarget screening by liquid chromatography–high-resolution mass spectrometry

Research output: Contribution to journalArticle

Abstract

Previous studies on organic sediment contaminants focused mainly on a limited number of highly hydrophobic micropollutants accessible to gas chromatography using nonpolar, aprotic extraction solvents. The development of liquid chromatography–high-resolution mass spectrometry (LC–HRMS) permits the spectrum of analysis to be expanded to a wider range of more polar and ionic compounds present in sediments and allows target, suspect, and nontarget screening to be conducted with high sensitivity and selectivity. In this study, we propose a comprehensive multitarget extraction and sample preparation method for characterization of sediment pollution covering a broad range of physicochemical properties that is suitable for LC–HRMS screening analysis. We optimized pressurized liquid extraction, cleanup, and sample dilution for a target list of 310 compounds. Finally, the method was tested on sediment samples from a small river and its tributaries. The results show that the combination of 100 °C for ethyl acetate–acetone (50:50, neutral extract) followed by 80 °C for acetone–formic acid (100:1, acidic extract) and methanol–10 mM sodium tetraborate in water (90:10, basic extract) offered the best extraction recoveries for 287 of 310 compounds. At a spiking level of 1 μg mL-1, we obtained satisfactory cleanup recoveries for the neutral extract—(93 ± 23)%—and for the combined acidic/basic extracts—(42 ± 16)%—after solvent exchange. Among the 69 compounds detected in environmental samples, we successfully quantified several pharmaceuticals and polar pesticides.

Details

Authors
  • Riccardo Massei
  • Harry Byers
  • Liza Marie Beckers
  • Jens Prothmann
  • Werner Brack
  • Tobias Schulze
  • Martin Krauss
Organisations
External organisations
  • Helmholtz Centre for Environmental Research
  • RWTH Aachen University
Research areas and keywords

Subject classification (UKÄ) – MANDATORY

  • Environmental Management
  • Analytical Chemistry

Keywords

  • High-resolution mass spectroscopy, Liquid chromatography, Multitarget screening, Pressurized liquid extraction, Sediments
Original languageEnglish
Number of pages12
JournalAnalytical and Bioanalytical Chemistry
StateE-pub ahead of print - 2017 Nov 3
Peer-reviewedYes