Detection of carbohydrates in sea ice extracellular polymeric substances via solid-phase extraction and HPLC-ESI-MS/MS

Rivaro, Paola; Ardini, Francisco; Grotti, Marco; Vivado, Davide; Salis, A.; Damonte, Gianluca

doi:10.1016/j.marchem.2020.103911

Cited by 7 publications

(7 citation statements)

References 27 publications

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“…The HPLC-ESI-MS/MS conditions were developed from those used in previous work for the identification of other organic iron ligands by slightly modifying the composition and gradient of the mobile phase [42]. The parameters evaluated in the method's setup (selectivity, linearity, LOD, and LOQ) resulted in adequate identification and the quantification of the two considered standard molecules.…”

Section: Discussionmentioning

confidence: 99%

A New Approach to Characterize Siderophore-Type Ligands in Seawater by Solid Phase Synthesis and SPE-HPLC-ESI-MS/MS Analysis

Rivaro,

Vivado,

Ianni

et al. 2024

JMSE

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Siderophores are organic ligands involved in dissolved iron (dFe) speciation in the oceans. Their study is crucial for a better understanding of the biogeochemical cycle of Fe in the marine environment, particularly in certain areas, such as the Southern Ocean, where Fe deficiency limits marine productivity. In this study, an analytical method is proposed for the extraction and pre-concentration of siderophores from seawater samples by solid phase extraction (SPE) and subsequent analysis by high-performance liquid chromatography—electrospray ionization—mass spectrometry (HPLC-ESI-MS/MS). Two siderophores were used as standards: Ferrioxamine E, a commercially available hydroxamate siderophore, and a staphyloferrin A-like compound with two citric acid units, synthesized in our laboratories by solid-phase peptide synthesis. A central composite design, considering different pH (2, 3.5, and 5) and sample loading volume (50, 125 and 200 mL) as variables, was used to optimize the extraction yield with SPE C18 cartridges. Tests were conducted on samples of artificial seawater spiked with siderophore standards. Ferrioxamine E showed high extraction yields in all tests carried out. On the contrary, the extraction of staphyloferrin A-like compound was significantly affected by both pH and loading volume.

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Section: Discussionmentioning

confidence: 99%

A New Approach to Characterize Siderophore-Type Ligands in Seawater by Solid Phase Synthesis and SPE-HPLC-ESI-MS/MS Analysis

Rivaro,

Vivado,

Ianni

et al. 2024

JMSE

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“…They are ubiquitous throughout sea ice on Earth and retained even in the absence of active cellular production (Deming et al 2017). The presence of compounds serving an analogous purpose to EPSs in extraterrestrial ice habitats could be assessed with mass spectrometry (MS) techniques and may help to inform instrument sensitivity requirements (Rivaro et al 2021).…”

Section: Search For Lifementioning

confidence: 99%

Subsurface Science and Search for Life in Ocean Worlds

et al. 2023

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Several worlds in our solar system are thought to hold oceans of liquid water beneath their frozen surfaces. These subsurface ice and ocean environments are promising targets in the search for life beyond Earth, but they also present significant new technical challenges to planetary exploration. With a focus on Jupiter’s moon Europa, here we (1) identify major benefits and challenges to subsurface ocean world science, (2) provide a multidisciplinary survey of relevant sample handling and life detection technologies, and (3) integrate those perspectives into the Subsurface Science and Search for Life in Ocean Worlds (SSSLOW) concept payload. We discuss scientific goals across three complementary categories: (1) search for life, (2) assess habitability, and (3) investigate geological processes. Major mission challenges considered include submerged operation in high-pressure environments, the need to sample fluids with a range of possible chemical conditions, and detection of biosignatures at low concentrations. The SSSLOW addresses these issues by tightly integrated instrumentation and sample handling systems to enable sequential, complementary measurements while prioritizing preservation of sample context. In this work, we leverage techniques and technologies across several fields to demonstrate a path toward future subsurface exploration and life detection in ice and ocean worlds.

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“…Seasonal process studies near continental or sea-ice melt (such as the Marginal Ice Zone) will allow us to capture the physical supply of Fe and ligands, in addition to the onset of spring blooms and subsequent biological depletion of resources. Additional parameters, including dissolved and particulate organic carbon, transparent exopolymeric particles (TEPs), and determination of ligand molecular structure via organic mass spectrometry (Rivaro et al, 2021), would benefit the identification of ligands from biological sources. Assessment of seafloor sediments to Fe and ligand supply requires collection of pore water samples for CLE-AdCSV analysis and measurements of diffusion and seawater movement at the seawater-sediment interface (i.e., Forsch et al, 2021).…”

Section: The Mertz Region and Southern Ocean Ligand Collectionmentioning

confidence: 99%

Identifying potential sources of iron-binding ligands in coastal Antarctic environments and the wider Southern Ocean

et al. 2022

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The availability of iron (Fe) to marine microbial communities is enhanced through complexation by ligands. In Fe limited environments, measuring the distribution and identifying the likely sources of ligands is therefore central to understanding the drivers of marine productivity. Antarctic coastal marine environments support highly productive ecosystems and are influenced by numerous sources of ligands, the magnitude of which varies both spatially and seasonally. Using competitive ligand exchange adsorptive cathodic stripping voltammetry (CLE-AdCSV) with 2-(2-thiazolylazo)-p-cresol (TAC) as a competing artificial ligand, this study investigates Fe-binding ligands (FeL) across the continental shelf break in the Mertz Glacier Region, East Antarctica (64 - 67°S; 138 - 154°E) during austral summer of 2019. The average FeL concentration was 0.86 ± 0.5 nM Eq Fe, with strong conditional stability constants (Log KFeL) averaging 23.1 ± 1.0. The strongest binding ligands were observed in modified circumpolar deep water (CDW), thought to be linked to bacterial Fe remineralisation and potential siderophore release. High proportions of excess unbound ligands (L’) were observed in surface waters, as a result of phytoplankton Fe uptake in the mixed layer and euphotic zone. However, FeL and L’ concentrations were greater at depth, suggesting ligands were supplied with dissolved Fe from upwelled CDW and particle remineralisation in benthic nepheloid layers over the shelf. Recent sea-ice melt appeared to support bacterial production in areas where Fe and ligands were exhausted. This study is included within our newly compiled Southern Ocean Ligand (SOLt) Collection, a database of publicly available Fe-binding ligand surveys performed south of 50°S. A review of the SOLt Collection brings attention to the paucity of ligand data collected along the East Antarctic coast and the difficulties in pinpointing sources of Fe and ligands in coastal environments. Elucidating poorly understood ligand sources is essential to predicting future Fe availability for microbial populations under rapid environmental change.

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Detection of carbohydrates in sea ice extracellular polymeric substances via solid-phase extraction and HPLC-ESI-MS/MS

Cited by 7 publications

References 27 publications

A New Approach to Characterize Siderophore-Type Ligands in Seawater by Solid Phase Synthesis and SPE-HPLC-ESI-MS/MS Analysis

A New Approach to Characterize Siderophore-Type Ligands in Seawater by Solid Phase Synthesis and SPE-HPLC-ESI-MS/MS Analysis

Subsurface Science and Search for Life in Ocean Worlds

Identifying potential sources of iron-binding ligands in coastal Antarctic environments and the wider Southern Ocean

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