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A new method for the determination of primary and secondary terrestrial and marine biomarkers in ice cores using liquid chromatography high-resolution mass spectrometry

King, Amy C.F. ORCID: https://orcid.org/0000-0002-1285-7568; Giorio, Chiara; Wolff, Eric; Thomas, Liz ORCID: https://orcid.org/0000-0002-3010-6493; Karroca, Ornela; Roverso, Marco; Schwikowski, Margit; Tapparo, Andrea; Gambaro, Andrea; Kalberer, Markus. 2019 A new method for the determination of primary and secondary terrestrial and marine biomarkers in ice cores using liquid chromatography high-resolution mass spectrometry. Talanta, 194. 233-242. https://doi.org/10.1016/j.talanta.2018.10.042

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This is a postprint version of an article published in Talanta. The final published version is available online at: https://doi.org/10.1016/j.talanta.2018.10.042
Revised Manuscript (for Open Access).docx - Accepted Version
Available under License Creative Commons Attribution Non-commercial No Derivatives 4.0.

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Abstract/Summary

The majority of atmospheric compounds measured in ice cores are inorganic, while analysis of their organic counterparts is a less well developed field. In recent years, understanding of formation, transport pathways and preservation of these compounds in ice and snow has improved, showing great potential for their use as biomarkers in ice cores. This study presents an optimised analytical technique for quantification of terrestrial and marine biosphere emissions of secondary organic aerosol (SOA) components and fatty acids in ice using HPLC-MS analysis. Concentrations of organic compounds in snow and ice are extremely low (typically ppb or ppt levels) and thus pre-concentration is required prior to analysis. Stir bar sorptive extraction (SBSE) showed potential for fatty acid compounds, but failed to recover SOA compounds. Solid phase extraction (SPE) recovered compounds across both organic groups but methods improving some recoveries came at the expense of others, and background contamination of fatty acids was high. Rotary evaporation was by far the best performing method across both SOA and fatty acid compounds, with average recoveries of 80%. The optimised preconcentration – HPLC-MS method achieved repeatability of 9% averaged for all compounds. In environmental samples, both concentrations and seasonal trends were observed to be reproducible when analysed in two different laboratories using the same method.

Item Type: Publication - Article
Digital Object Identifier (DOI): https://doi.org/10.1016/j.talanta.2018.10.042
ISSN: 00399140
Additional Keywords: Ice core, Biomarker, Organic Aerosol, Liquid Chromatography, Mass Spectrometry, Paleoclimate
Date made live: 14 Feb 2019 11:13 +0 (UTC)
URI: https://nora.nerc.ac.uk/id/eprint/521462

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