Online supercritical fluid extraction mass spectrometry (SFE-LC-FTMS) for sensitive characterization of soil organic matter

Shen, Yufeng; Zhao, Rui; Tolić, Nikola; Tfaily, Malak M.; Robinson, Errol W.; Boiteau, Rene; Paša-Tolić, Ljiljana; Hess, Nancy J.

doi:10.1039/C9FD00011A

Title: Online supercritical fluid extraction mass spectrometry (SFE-LC-FTMS) for sensitive characterization of soil organic matter

Journal Article · Mon Mar 25 00:00:00 EDT 2019 · Faraday Discussions

DOI:https://doi.org/10.1039/C9FD00011A· OSTI ID:1573023

Shen, Yufeng ^[1]; Zhao, Rui ^[2];

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Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Biological Sciences Division; CoAnn Technologies, Richland, WA (United States)
Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Environmental Molecular Sciences Lab. (EMSL)
Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Environmental Molecular Sciences Lab. (EMSL); Univ. of Arizona, Tucson, AZ (United States). Dept. of Soil, Water and Environmental Science
Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Biological Sciences Division
Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Environmental Molecular Sciences Lab. (EMSL); Oregon State Univ., Corvallis, OR (United States). College of Earth, Ocean and Atmospheric Sciences

We report a novel technical approach for subcritical fluid extraction (SFE) for organic matter characterization in complex matrices such as soil. The custom platform combines on-line SFE with micro-solid phase extraction, nano liquid chromatography (LC), electrospray ionization and Fourier transform mass spectrometry (SFE-LC-FTMS). We demonstrated the utility of SFE-LC-FTMS, including results from both Orbitrap and FTICR MS, for analysis of complex mixtures of organic compounds in a solid matrix by characterizing soil organic matter in peat, a high-carbon soil. For example, in a single experiment, >6000 molecular formulas can be assigned based upon FTICR MS data from 1–50 μL of soil samples (roughly 1–50 mg of soil, dependent on soil density), nearly twice that typically obtained from direct infusion liquid solvent extraction (LSE) from an order of magnitude larger volume of the same soil. The detected species consisted predominately of lipid-like, lignin-like and protein-like compounds, based on their O/C and H/C ratios, with predominantly CHO and CHONP molecular compositions. These results clearly demonstrate that SFE has the potential to effectively extract a variety of molecular species and could become an important member of a suite of extraction methods for studying SOM and other natural organic matter. This is especially true when comprehensive coverage, minimal sample volumes, and high sensitivity are required, or when the presence of organic solvent residue in residual soil is problematic. Lastly, the SFE based extraction protocol could potentially enable spatially resolved characterization of organic matter in soil with a resolution of ~1 mm3 to facilitate studies probing the spatial heterogeneity of soil.

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Research Organization:: Pacific Northwest National Laboratory (PNNL), Richland, WA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Biological and Environmental Research (BER)

Grant/Contract Number:: AC05-76RL01830

OSTI ID:: 1573023

Alternate ID(s):: OSTI ID: 1524103

Report Number(s):: PNNL-SA-141115; FDISE6

Journal Information:: Faraday Discussions, Vol. 218; ISSN 1359-6640

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 5 works

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54 ENVIRONMENTAL SCIENCES
supercritical fluid extraction (SFE)
liquid chromatography (LC)
electrospray ionization (ESI)
Fourier transform mass spectrometry (FTMS)
Fourier transform ion cyclotron resonance (FTICR)
soil organic matter (SOM)

Title: Online supercritical fluid extraction mass spectrometry (SFE-LC-FTMS) for sensitive characterization of soil organic matter

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