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Stoichiometry between Humate Unit Molecules and Metal Ions in Supramolecular Assembly Induced by Cu2+ and Tb3+ Measured by Gel Electrophoresis Techniques
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    Contaminants in Aquatic and Terrestrial Environments

    Stoichiometry between Humate Unit Molecules and Metal Ions in Supramolecular Assembly Induced by Cu2+ and Tb3+ Measured by Gel Electrophoresis Techniques
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    • Sumika Nakano
      Sumika Nakano
      Graduate School of Science and Engineering, Saitama University, 255 Shimo-Okubo, Sakura-ku, Saitama 338-8570, Japan
    • Kazuki Marumo
      Kazuki Marumo
      Graduate School of Science and Engineering, Saitama University, 255 Shimo-Okubo, Sakura-ku, Saitama 338-8570, Japan
    • Rintaro Kazami
      Rintaro Kazami
      Graduate School of Science and Engineering, Saitama University, 255 Shimo-Okubo, Sakura-ku, Saitama 338-8570, Japan
    • Takumi Saito
      Takumi Saito
      Nuclear Professional School, Graduate School of Engineering, The University of Tokyo, 2-21 Shirakata-Shirane, Tokai-mura, Ibaraki 319-1188, Japan
      More by Takumi Saito
    • Tomoko Haraga
      Tomoko Haraga
      Department of Decommissioning and Waste Management, Japan Atomic Energy Agency, 2-4 Shirakata, Tokai-mura, Naka-gun, Ibaraki 319-1195, Japan
    • Yuiko Tasaki-Handa
      Yuiko Tasaki-Handa
      Graduate School of Science and Engineering, Saitama University, 255 Shimo-Okubo, Sakura-ku, Saitama 338-8570, Japan
    • Shingo Saito*
      Shingo Saito
      Graduate School of Science and Engineering, Saitama University, 255 Shimo-Okubo, Sakura-ku, Saitama 338-8570, Japan
      *Email: [email protected]. Phone: +81 48 858 3559.
      More by Shingo Saito
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    Environmental Science & Technology

    Cite this: Environ. Sci. Technol. 2021, 55, 22, 15172–15180
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    https://doi.org/10.1021/acs.est.1c03993
    Published November 3, 2021
    Copyright © 2021 American Chemical Society

    Abstract

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    Humic acid (HA), a fraction of humic substances, can strongly complex with metal ions to form a supramolecular assembly via coordination binding and other intermolecular forces. However, determining the supramolecular size distribution and stoichiometry between small HA unit molecules constituting HA supramolecules and metal ions has proven to be challenging. Here, we investigated the changes in the size distributions of HAs induced by Cu2+ and Tb3+ ions using unique PAGE for the separation and quantification of HA complexes and metal ions bound, followed by UV–vis spectroscopy and excitation–emission matrix–parallel factor analysis. By determining the concentrations of HA and metal ions, it was possible to estimate the stoichiometry of the HA unit molecule to metal ions in supramolecular complexes. It was found that the supramolecular behaviors of Cu2+ and Tb3+ complexes with HA collected from peat (PAHA) and deep groundwater (HHA) differed. For example, two HHA unit molecules form a supramolecule via cross-linking by a Cu2+ ion in the case of Cu2+–HHA. Our results suggest that this supramolecular stoichiometry is related to the abundance of sulfur atoms in the elemental composition of HHA. Our experimental results and analysis provide new insights into HA supramolecules formed via metal complexation.

    Copyright © 2021 American Chemical Society

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    Supporting Information

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    The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acs.est.1c03993.

    • Methods of EEM–PARAFAC, composition ratio, and acidic functional groups, results of metal detection PAGE of Ln3+ using the fluorescent probe, results of PARAFAC modeling of EEM data, and MW distribution of metal–HA complexes (PDF)

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    This article is cited by 5 publications.

    1. Kazuhito Yamagata, Kazuki Ouchi, Kazuki Marumo, Yuiko Tasaki-Handa, Tomoko Haraga, Shingo Saito. Unusually Kinetically Inert Monocationic Neptunyl Complex with a Fluorescein-Modified 1,10-Phenanthroline-2,9-dicarboxylate Ligand: Specific Separation and Detection in Gel Electrophoresis. Inorganic Chemistry 2023, 62 (2) , 730-738. https://doi.org/10.1021/acs.inorgchem.2c02908
    2. Shingo Saito, Junko Ishikawa, Moe Ono, Yuiko Tasaki-Handa, Masami Shibukawa. Holo/apo conversion two-dimensional urea PAGE for speciation of Fe3+-bound transferrin in serum. Analytical Sciences 2024, 40 (2) , 227-233. https://doi.org/10.1007/s44211-023-00460-z
    3. Xiaolei Liu, Bin Ji, Anjie Li. Enhancing biolipid production and self-flocculation of Chlorella vulgaris by extracellular polymeric substances from granular sludge with CO2 addition: Microscopic mechanism of microalgae-bacteria symbiosis. Water Research 2023, 236 , 119960. https://doi.org/10.1016/j.watres.2023.119960
    4. Shingo Saito, Tomoko Haraga, Kazuki Marumo, Yoshiyuki Sato, Yuta Nakano, Yuiko Tasaki-Handa, Masami Shibukawa. Americium(III)/Curium(III) Complete Separation and Sensitive Fluorescence Detection by Capillary and Gel Electrophoresis Using Emissive Hexadentate/Octadentate Polyaminocarboxylate Ligands. Bulletin of the Chemical Society of Japan 2023, 96 (3) , 223-225. https://doi.org/10.1246/bcsj.20220346
    5. Shingo Saito. Separation approaches towards understanding supramolecular aggregate formation of humic acid. Analytical Sciences 2022, 38 (2) , 233-234. https://doi.org/10.1007/s44211-021-00020-3

    Environmental Science & Technology

    Cite this: Environ. Sci. Technol. 2021, 55, 22, 15172–15180
    Click to copy citationCitation copied!
    https://doi.org/10.1021/acs.est.1c03993
    Published November 3, 2021
    Copyright © 2021 American Chemical Society

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