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Analysis of estrogens in river sediments using liquid chromatography-electrospray ionization mass spectrometry: Comparision of tandem mass spectrometry with time-of-flight mass spectrometry
journal contribution
posted on 2023-06-08, 00:45 authored by Pierre Labadie, Elizabeth M HillA method has been developed and optimised for the determination of two natural estrogens, estrone (E1) and 17beta-estradiol (E2), and one synthetic estrogen, 17alpha-ethynylestradiol (EE2), in river sediments at the sub-ng/g level. This procedure includes microwave-assisted solvent extraction (MASE), solid-phase extraction and high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) with electrospray ionisation. Using sediments spiked with the three estrogens at 10 ng/g wet weight, efficient extraction (>92%) of all the three analytes was achieved by MASE, and whole-procedure recoveries ranged from 82 to 98%. Optimisation of the LC separation allowed for substantial reduction of ionisation suppression in the electrospray source to a final level of <18% suppression. Time-of-flight mass spectrometry (TOF-MS) and MS/MS were compared for the analysis of sediment extracts, with the latter technique proving to be the most selective. The method detection limits achieved by LC-MS/MS were 15, 30 and 40 pg/g for E1, E2 and EE2, respectively, which were 13-fold lower than those obtained by LC-TOF-MS. Analysis of river sediments collected from the River Ouse, UK, showed the presence of the natural estrogens at sub-ng/g level. E1 levels ranged from 0.40 ng/g (dry weight) to 3.30 ng/g while E2 levels ranged from <0.03 to 1.20 ng/g and EE2 was never detected (<0.04 ng/g).
History
Publication status
- Published
Journal
Journal of Chromatography AISSN
0021-9673Publisher
ElsevierExternal DOI
Issue
2Volume
1141Page range
174-181Pages
8.0Department affiliated with
- Evolution, Behaviour and Environment Publications
Full text available
- No
Peer reviewed?
- Yes
Legacy Posted Date
2012-02-06Usage metrics
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