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Solvent-selective complexity reduction of effluent dissolved organic matter for 1H NMR spectroscopy
Department of Thematic Studies - Environmental Change, Linköping University, Linköping, Sweden; Biogas Solutions Research Center, Linköping University, Linköping, Sweden.
Department of Thematic Studies - Environmental Change, Linköping University, Linköping, Sweden; Biogas Solutions Research Center, Linköping University, Linköping, Sweden.
Umeå University, Faculty of Science and Technology, Department of Chemistry.ORCID iD: 0000-0002-0903-6662
Umeå University, Faculty of Science and Technology, Department of Chemistry.
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2026 (English)In: Analytical Chemistry, ISSN 0003-2700, E-ISSN 1520-6882, Vol. 98, no 15, p. 11149-11157Article in journal (Refereed) Published
Abstract [en]

Processing of biomass residues for material and energy recovery generate effluents containing complex organic mixtures. Analyses of bulk parameters are conventional for characterization and classification of such effluents, where the limited information offered impedes the development of molecular level management practices. This study assessed the potential of solvent-selective complexity reduction of effluent dissolved organic matter (DOM) from anaerobic bioprocessing of biomass residues for 1H NMR spectroscopy. The DOM were acquired after filtration and drying of samples from seven full scale anaerobic bioreactor facilities with effluents used as biofertilizer. The 1H NMR spectra of DOM in indigenous solvent (water) revealed source dependent characteristics primarily due to variable abundance of aliphatic CCH in lipids and peptides, OCCH in carbohydrates, and olefinic and aromatic subunits. Dimethyl sulfoxide solubilized larger proportion of nonfunctionalized aliphatic and aromatic molecules, with 1H NMR features also varying depending on the DOM source. Methanol, however, reduced the 1H NMR spectral variability and dissolved sets of aliphatic and aromatic molecules from the dried DOM with similar 1H NMR features irrespective of their origin. Among the other solvents studied, the reactive dissolution by trifluoroacetic acid decomposed aliphatic units while enriching aromatics (i.e., CarH:CCH of 0.7 compared to 0.2 in water), also forming small (oligo)saccharides and peptide fragments. Acetone, dichloromethane, and acetonitrile extracted alkyl-rich molecules with varying degrees of functionalization. Acetonitrile separated a fraction enriched in aliphatic carboxylic acids, while dichloromethane mainly dissolved nonfunctionalized aliphatic hydrocarbons. It is proposed that a simple process of filtration, drying, and dissolution of effluent DOM in different solvents substantially reduces the complexity and heterogeneity of the organic mixtures enabling the structural discrimination of diverse molecular classes by 1H NMR spectroscopy.

Place, publisher, year, edition, pages
American Chemical Society (ACS), 2026. Vol. 98, no 15, p. 11149-11157
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Organic Chemistry Physical Chemistry
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URN: urn:nbn:se:umu:diva-252784DOI: 10.1021/acs.analchem.5c07560ISI: 001734640800001PubMedID: 41943596Scopus ID: 2-s2.0-105036532894OAI: oai:DiVA.org:umu-252784DiVA, id: diva2:2061803
Funder
Swedish Energy Agency, 35624-2Swedish Energy Agency, P2021-90266ÅForsk (Ångpanneföreningen's Foundation for Research and Development), 23-259Available from: 2026-05-22 Created: 2026-05-22 Last updated: 2026-05-22Bibliographically approved

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Hedenström, MattiasSparrman, Tobias

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