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

Massei, Riccardo; Byers, Harry; Beckers, Liza Marie; Prothmann, Jens LU ; Brack, Werner; Schulze, Tobias and Krauss, Martin (2017) In Analytical and Bioanalytical Chemistry
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... (More)

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.

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author
organization
publishing date
type
Contribution to journal
publication status
epub
subject
keywords
High-resolution mass spectroscopy, Liquid chromatography, Multitarget screening, Pressurized liquid extraction, Sediments
in
Analytical and Bioanalytical Chemistry
pages
12 pages
publisher
Springer
external identifiers
  • scopus:85032833506
ISSN
1618-2642
DOI
10.1007/s00216-017-0708-9
language
English
LU publication?
yes
id
a3d86c8f-e4c0-421e-bee0-39f624f2a2ba
date added to LUP
2017-11-14 13:24:48
date last changed
2017-11-15 03:00:03
@article{a3d86c8f-e4c0-421e-bee0-39f624f2a2ba,
  abstract     = {<p>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<sup>-1</sup>, 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.</p>},
  author       = {Massei, Riccardo and Byers, Harry and Beckers, Liza Marie and Prothmann, Jens and Brack, Werner and Schulze, Tobias and Krauss, Martin},
  issn         = {1618-2642},
  keyword      = {High-resolution mass spectroscopy,Liquid chromatography,Multitarget screening,Pressurized liquid extraction,Sediments},
  language     = {eng},
  month        = {11},
  pages        = {12},
  publisher    = {Springer},
  series       = {Analytical and Bioanalytical Chemistry},
  title        = {A sediment extraction and cleanup method for wide-scope multitarget screening by liquid chromatography–high-resolution mass spectrometry},
  url          = {http://dx.doi.org/10.1007/s00216-017-0708-9},
  year         = {2017},
}