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Molecular Tracers and Untargeted Characterization of Water Soluble Organic Compounds in Polar Ice for Climate Change Studies

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Molecular Tracers and Untargeted Characterization of Water Soluble Organic Compounds in Polar Ice for Climate Change Studies PhD Thesis in SCIENCE AND MANAGEMENT OF CLIMATE CHANGE Molecular tracers and untargeted characterization of water soluble organic compounds in polar ice for climate change studies. PhD Candidate Ornela Karroca Supervisor Prof. Andrea Gambaro Co-Supervisor Dr. Roberta Zangrando 1 GLOSSARY 1. ABSTRACT ........................................................................................................................................ 4 2. INTRODUCTION ............................................................................................................................... 5 3. THESIS GOALS ................................................................................................................................ 15 4. EXPERIMENTAL SECTION ............................................................................................................... 16 4.1 Reagents and standard solutions ............................................................................................ 16 4.2 Quantitative analyses .............................................................................................................. 17 4.2.1 Instrumentation and working conditions .......................................................................... 17 4.2.2 Amino acids and phenolic compounds: Method validation .............................................. 21 4.2.2.1 Chromatographic separation ..................................................................................... 21 4.2.2.2 Quality control............................................................................................................ 22 4.2.3 Quantitative analyses of amino acids and phenolic compounds in Talos Dome samples . 28 4.2.3.1 Talos Dome site .......................................................................................................... 28 4.2.3.2 Sample preeparation .................................................................................................. 36 4.2.4 Quantitative analyses of amino acids in Renland samples .............................................. 37 4.2.4.1 Talos Dome site .......................................................................................................... 37 4.2.4.2 Talos Dome site .......................................................................................................... 39 4.3 Preconcentration of fatty acids and atmospheric markers: Method optimization .............. 40 4.3.1 Rendezvous site ................................................................................................................. 40 4.3.2 Instrumentation and working conditions .......................................................................... 41 4.3.3 Sample preparation .......................................................................................................... 44 4.4 Qualitative analyses ................................................................................................................ 45 4.4.1 Instrumentation ................................................................................................................ 45 4.4.2 A preliminary qualitative analysis with UHPLC-ESI/MS method ...................................... 46 4.4.2.1 Sample preparation .................................................................................................... 46 2 4.4.2.2 Working conditions ................................................................................................... 47 4.4.3 Qualitative analyses nanoUHPLC-nanoESI/MS method ................................................... 52 4.4.3.1 Working conditions .................................................................................................... 52 4.5 Data elaboration ...................................................................................................................... 54 4.5.1 Quantitative analyses ....................................................................................................... 54 4.5.2 Qualitative analyses .......................................................................................................... 56 5. RESULTS AND DISCUSSIONS .......................................................................................................... 63 5.1 Phenolic compounds and amino acids in Talos Dome ice core ............................................. 63 5.2 Amino acids in Renland ice core ............................................................................................. 70 5.3 Qualitative analyses of Talos Dome samples ......................................................................... 76 6. CONCLUSIONS ................................................................................................................................ 88 7. SUPPLEMENTARY MATERIAL ........................................................................................................ 91 8. BIBLIOGRAPHY ............................................................................................................................. 119 3 1. ABSTRACT The polar regions are an excellent archive of past atmospheric conditions rendering polar ice investigation extremely important for paleoclimate studies. The presence of organic compounds, such as amino acids and methoxyphenol compounds, could lead to important insights regarding the presence of past biological material and biomass burning information, respectively. Amino acids constitute an important fraction of organic matter, as well as a source of carbon, nitrogen and energy. Moreover, L-amino acids are the most common enantiomer present in nature and are indicative of phytoplanktonic material: on the other hand, D-amino acids are linked to the presence of bacteria. With the aim of detecting possible past bacterial presence, we investigated both D- and L-amino acid enantiomers in two ice cores: Talos Dome, East Antarctica, and Renland, Eastern Greenland. In selected Talos Dome ice core samples was performed a qualitative analysis to detect the chemical composition and to investigate the past and/or ongoing chemical transformations of the chemical species found. Phenolic compounds are produced by lignin combustion and are specific molecular markers used to assess combustion sources. For this purpose, their presence was investigated in the Talos Dome ice core samples. For both, amino acids (D-/L- enantiomers) and methoxyphenols, were validated the respective analytical methods. Moreover, specific quality control assessments for each analyte were performed. A part of this work was focused on the optimization of a preconcentration analytical method for several fatty acids and atmospheric markers. The preconcentration preliminary step was performed in order to be applicable to real ice and snow samples, with the purpose to ensure the detection of low concentrations with the disposable instruments. The presence of fatty acids provide important information since are mainly derived by phospholipids and triglycerides, which are accumulated during algal bloom, giving insights on the biological activity of the surrounding marine ecosystems. 4 2. INTRODUCTION The polar ice is often used to extract paleoclimatic information since is considered to be a storage of past atmospheric composition. The snow deposition, in absence of snow melting, reflects the past atmospheric composition in polar regions allowing the deposition and conservation of important atmospheric markers. Moreover, the distance from anthropogenic sources makes the polar regions important for investigating the natural sources of atmospheric aerosol (Barbaro et al., 2017). Given the importance in terms of paleoclimate studies of polar ice matrices, as well as the low concentrations of atmospheric tracers archived in it, becomes fundamental the optimization of the analytical techniques used for the detection of atmospheric markers present in traces in order to achieve the highest sensitivity. The study of these markers is essential to detect specific environmental processes, such as biomass burning, investigating on the presence of levoglucosan and phenolic compounds, and primary production studying the presence of amino acid species. For this reason, during this thesis one of the main purposes was the development of a sensitive analytical method and the detection of amino acid and phenolic compounds in Antarctic and Arctic ice samples. The amino acid compounds are studied widely in this thesis since represent a source of carbon, nitrogen and energy, and constitute a part of organic matter in marine and freshwater ecosystems. Amino acids are used by bacteria and phytoplankton species as a source of nitrogen and are released from soil organic matter, as well as by terrestrial plants, living phytoplankton and cellular lysis of senescent algae. They also play an important role in the carbon flux acting as intermediates, although they represent a small part of the total dissolved organic carbon due to the low concentrations (Berman and Bronk, 2003; Bronk et al., 1994). In past studies were performed analyses of amino acids in other environmental matrices, other than in polar ice as performed in this work, such as in seawater with early studies (Belser 1959; Tatsumoto et al., 1961; Palmark, 1963) followed by more recent works, and in atmospheric aerosols (Barbaro et al., 2015; Matos et al., 2016), since the amino acid compounds are an important component of organic nitrogen in 5 atmospheric aerosols (Chan et al. 2005). The aim of our work is to collect
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