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Category Text Publication
Reference Category Journals
DOI 10.1007/s00216-017-0708-9
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Title (Primary) A sediment extraction and cleanup method for wide-scope multitarget screening by liquid chromatography–high-resolution mass spectrometry
Author Massei, R.; Byers, H.; Beckers, L.-M.; Prothmann, J.; Brack, W.; Schulze, T. ORCID logo ; Krauss, M. ORCID logo
Source Titel Analytical and Bioanalytical Chemistry
Year 2018
Department WANA
Volume 410
Issue 1
Page From 177
Page To 188
Language englisch
Supplements https://static-content.springer.com/esm/art%3A10.1007%2Fs00216-017-0708-9/MediaObjects/216_2017_708_MOESM1_ESM.pdf
https://static-content.springer.com/esm/art%3A10.1007%2Fs00216-017-0708-9/MediaObjects/216_2017_708_MOESM2_ESM.xlsx
Keywords Sediments; Liquid chromatography; High-resolution mass spectroscopy; Multitarget screening; Pressurized liquid extraction
UFZ wide themes RU3;
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.
Persistent UFZ Identifier https://www.ufz.de/index.php?en=20939&ufzPublicationIdentifier=19797
Massei, R., Byers, H., Beckers, L.-M., Prothmann, J., Brack, W., Schulze, T., Krauss, M. (2018):
A sediment extraction and cleanup method for wide-scope multitarget screening by liquid chromatography–high-resolution mass spectrometry
Anal. Bioanal. Chem. 410 (1), 177 - 188 10.1007/s00216-017-0708-9