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Online supercritical fluid extraction mass spectrometry (SFE-LC-FTMS) for sensitive characterization of soil organic matter.
Shen, Yufeng; Zhao, Rui; Tolic, Nikola; Tfaily, Malak M; Robinson, Errol W; Boiteau, Rene; Pasa-Tolic, Ljiljana; Hess, Nancy J.
Afiliação
  • Shen Y; Biological Sciences Division, Pacific Northwest National Laboratory, Richland, WA 99354, USA.
Faraday Discuss ; 218(0): 157-171, 2019 08 15.
Article em En | MEDLINE | ID: mdl-31155623
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. 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.

Texto completo: 1 Coleções: 01-internacional Base de dados: MEDLINE Tipo de estudo: Diagnostic_studies Idioma: En Ano de publicação: 2019 Tipo de documento: Article

Texto completo: 1 Coleções: 01-internacional Base de dados: MEDLINE Tipo de estudo: Diagnostic_studies Idioma: En Ano de publicação: 2019 Tipo de documento: Article