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Analytical and Bioanalytical Chemistry

, Volume 411, Issue 10, pp 2201–2208 | Cite as

Separation and characterization of marine dissolved organic matter (DOM) by combination of Fe(OH)3 co-precipitation and solid phase extraction followed by ESI FT-ICR MS

  • Lijie LiEmail author
  • Zhi Fang
  • Chen He
  • Quan Shi
Research Paper

Abstract

Marine dissolved organic matter (DOM) constitutes a major carbon pool in the global carbon cycle. Characterization of its chemical composition will improve our understanding of its role in global biogeochemical cycles. Currently, solid phase extraction (SPE) followed by Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) analysis has become a powerful approach to characterize the molecular composition of DOM. However, some components in marine DOM, such as highly oxygenated tannin-like molecules, were lost during the SPE process. In this study, a sequential combination of co-precipitation and SPE procedure was proposed to improve the yield of marine DOM extraction. Ferric hydroxide was used as the co-precipitation agent to separate marine DOM, and SPE was carried out for the extraction of DOM from dissolved and precipitate fractions. The total yield in total organic carbon (TOC) and the number of assigned molecules of SPE-DOM increased by 25% and 51%, respectively, compared with those by direct SPE process. The combined process has good selectivity on tannin-like compounds. The result is instructive for the understanding of DOM molecular composition and potential for a routine method for DOM extraction from environmental water samples, especially for marine DOM containing a small amount of tannin-like compounds.

Keywords

Dissolved organic matter Co-precipitation SPE FT-ICR MS 

Notes

Funding information

This work was supported by the National Key Research and Development Program of China (2018YFA0605800).

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.

Supplementary material

216_2019_1663_MOESM1_ESM.pdf (741 kb)
ESM 1 (PDF 740 kb)

References

  1. 1.
    Siegenthaler U, Sarmiento J. Atmospheric carbon dioxide and the ocean. Nature. 1993;365(6442):119–25.CrossRefGoogle Scholar
  2. 2.
    Sexton PF, Norris RD, Wilson PA, Pälike H, Westerhold T, Röhl U, et al. Eocene global warming events driven by ventilation of oceanic dissolved organic carbon. Nature. 2011;471(7338):349–52.CrossRefGoogle Scholar
  3. 3.
    Derenne S, Tu TTN. Characterizing the molecular structure of organic matter from natural environments: an analytical challenge. Compt Rendus Geosci. 2014;346(3–4):53–63.CrossRefGoogle Scholar
  4. 4.
    Dittmar T, Koch B, Hertkorn N, Kattner G. A simple and efficient method for the solid-phase extraction of dissolved organic matter (SPE-DOM) from seawater. Limnol Oceanogr Methods. 2008;6(6):230–5.CrossRefGoogle Scholar
  5. 5.
    McDonald S, Bishop A, Prenzler P, Robards K. Analytical chemistry of freshwater humic substances. Anal Chim Acta. 2004;527(2):105–24.CrossRefGoogle Scholar
  6. 6.
    Murphy KR, Stedmon CA, Waite TD, Ruiz GM. Distinguishing between terrestrial and autochthonous organic matter sources in marine environments using fluorescence spectroscopy. Mar Chem. 2008;108(1–2):40–58.CrossRefGoogle Scholar
  7. 7.
    Miller MP, McKnight DM. Comparison of seasonal changes in fluorescent dissolved organic matter among aquatic lake and stream sites in the Green Lakes Valley. J Geophys Res Biogeosci. 2010;115(G1):91–103.Google Scholar
  8. 8.
    Minor E, Stephens B. Dissolved organic matter characteristics within the Lake Superior watershed. Org Geochem. 2008;39(11):1489–501.CrossRefGoogle Scholar
  9. 9.
    Li C, Benjamin MM, Korshin GV. Use of UV spectroscopy to characterize the reaction between NOM and free chlorine. Environ Sci Technol. 2000;34(12):2570–5.CrossRefGoogle Scholar
  10. 10.
    Abdulla HAN, Minor EC, Hatcher PG. Using two-dimensional correlations of 13C NMR and FTIR to investigate changes in the chemical composition of dissolved organic matter along an estuarine transect. Environ Sci Technol. 2010;44(21):8044–9.CrossRefGoogle Scholar
  11. 11.
    Abdulla HAN, Minor EC, Dias RF, Hatcher PG. Changes in the compound classes of dissolved organic matter along an estuarine transect: a study using FTIR and 13C NMR. Geochim Cosmochim Acta. 2010;74(13):3815–38.  https://doi.org/10.1016/j.gca.2010.04.006.CrossRefGoogle Scholar
  12. 12.
    Cook RL. Coupling NMR to NOM. Anal Bioanal Chem. 2004;378(6):1484–503.CrossRefGoogle Scholar
  13. 13.
    Sutton R, Sposito G. Molecular structure in soil humic substances: the new view. Environ Sci Technol. 2005;39(23):9009–15.CrossRefGoogle Scholar
  14. 14.
    Koch BP, Dittmar T, Matthias Witt A, Kattner G. Fundamentals of molecular formula assignment to ultrahigh resolution mass data of natural organic matter. Anal Chem. 2007;79(4):1758–63.CrossRefGoogle Scholar
  15. 15.
    Ruddy BM, Hendrickson CL, Rodgers RP, Marshall AG. Positive ion electrospray ionization suppression in petroleum and complex mixtures. Energy Fuel. 2018;32(3):2901–7.CrossRefGoogle Scholar
  16. 16.
    Li Y, Xu C, Chung KH, Shi Q. Molecular characterization of dissolved organic matter and its subfractions in refinery process water by Fourier transform ion cyclotron resonance mass spectrometry. Energy Fuel. 2015;29(5):2923–30.CrossRefGoogle Scholar
  17. 17.
    Zhang HF, Zhang YH, Shi Q, Zheng HD, Yang M. Characterization of unknown brominated disinfection byproducts during chlorination using ultrahigh resolution mass spectrometry. Environ Sci Technol. 2014;48(6):3112–9.  https://doi.org/10.1021/es4057399.CrossRefGoogle Scholar
  18. 18.
    Zhang HF, Zhang YH, Shi Q, Hu JY, Chu MQ, Yu JW, et al. Study on transformation of natural organic matter in source water during chlorination and its chlorinated products using ultrahigh resolution mass spectrometry. Environ Sci Technol. 2012;46(8):4396–402.  https://doi.org/10.1021/es203587q.CrossRefGoogle Scholar
  19. 19.
    Li Y, Harir M, Lucio M, Gonsior M, Koch BP, Schmitt-Kopplin P, et al. Comprehensive structure-selective characterization of dissolved organic matter by reducing molecular complexity and increasing analytical dimensions. Water Res. 2016;106:477–87.CrossRefGoogle Scholar
  20. 20.
    Yuan Z, He C, Shi Q, Xu C, Li Z, Wang C, et al. Molecular insights into the transformation of dissolved organic matter in landfill leachate concentrate during biodegradation and coagulation processes using ESI FT-ICR MS. Environ Sci Technol. 2017;51(14):8110–8.CrossRefGoogle Scholar
  21. 21.
    Sleighter RL, Hatcher PG. Molecular characterization of dissolved organic matter (DOM) along a river to ocean transect of the lower Chesapeake Bay by ultrahigh resolution electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry. Mar Chem. 2008;110(3):140–52.CrossRefGoogle Scholar
  22. 22.
    Reemtsma T, These A, Linscheid M, Leenheer J, Spitzy A. Molecular and structural characterization of dissolved organic matter from the deep ocean by FTICR-MS, including hydrophilic nitrogenous organic molecules. Environ Sci Technol. 2008;42(5):1430–7.CrossRefGoogle Scholar
  23. 23.
    Patriarca C, Bergquist J, Sjöberg PJR, Tranvik L, Hawkes JA. Online HPLC-ESI-HRMS method for the analysis and comparison of different dissolved organic matter samples. Environ Sci Technol. 2017;52(4):2091–9.CrossRefGoogle Scholar
  24. 24.
    Fang Z, He C, Li Y, Chung KH, Xu C, Shi Q. Fractionation and characterization of dissolved organic matter (DOM) in refinery wastewater by revised phase retention and ion-exchange adsorption solid phase extraction followed by ESI FT-ICR MS. Talanta. 2017;162:466–73.CrossRefGoogle Scholar
  25. 25.
    Li Y, Fang Z, He C, Zhang Y, Xu C, Chung KH, et al. Molecular characterization and transformation of dissolved organic matter in refinery wastewater from water treatment processes: characterization by Fourier transform ion cyclotron resonance mass spectrometry. Energy Fuel. 2015;29(11):6956–63.CrossRefGoogle Scholar
  26. 26.
    Shi Q, Hou D, Chung KH, Xu C, Zhao S, Zhang Y. Characterization of heteroatom compounds in a crude oil and its saturates, aromatics, resins, and asphaltenes (SARA) and non-basic nitrogen fractions analyzed by negative-ion electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry. Energy Fuel. 2010;24(4):2545–53.CrossRefGoogle Scholar
  27. 27.
    Liu P, Shi Q, Chung KH, Zhang Y, Pan N, Zhao S, et al. Molecular characterization of sulfur compounds in Venezuela crude oil and its SARA fractions by electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry. Energy Fuel. 2010;24(9):5089–96.CrossRefGoogle Scholar
  28. 28.
    Kleint C, Pichler T, Koschinsky A. Geochemical characteristics, speciation and size-fractionation of iron (Fe) in two marine shallow-water hydrothermal systems, Dominica, Lesser Antilles. Chem Geol. 2017;454:44–53.CrossRefGoogle Scholar
  29. 29.
    Linkhorst A, Dittmar T, Waska H. Molecular fractionation of dissolved organic matter in a shallow subterranean estuary: the role of the iron curtain. Environ Sci Technol. 2016;51(3):1312–20.CrossRefGoogle Scholar
  30. 30.
    Gomez-Saez GV, Riedel T, Niggemann J, Pichler T, Dittmar T, Bühring SI. Interaction between iron and dissolved organic matter in a marine shallow hydrothermal system off Dominica Island (Lesser Antilles). Mar Chem. 2015;177:677–86.CrossRefGoogle Scholar
  31. 31.
    Riedel T, Zak D, Biester H, Dittmar T. Iron traps terrestrially derived dissolved organic matter at redox interfaces. Proc Natl Acad Sci U S A. 2013;110(25):10101–5.CrossRefGoogle Scholar
  32. 32.
    Li Y, Harir M, Lucio M, Kanawati B, Smirnov K, Flerus R, et al. Proposed guidelines for solid phase extraction of Suwannee River dissolved organic matter. Anal Chem. 2016;88(13):6680–8.CrossRefGoogle Scholar
  33. 33.
    Lv J, Zhang S, Wang S, Luo L, Cao D, Christie P. Molecular-scale investigation with ESI-FT-ICR-MS on fractionation of dissolved organic matter induced by adsorption on iron oxyhydroxides. Environ Sci Technol. 2016;50(5):2328–36.CrossRefGoogle Scholar
  34. 34.
    Riedel T, Biester H, Dittmar T. Molecular fractionation of dissolved organic matter with metal salts. Environ Sci Technol. 2012;46(8):4419–26.CrossRefGoogle Scholar
  35. 35.
    Stenson AC. Reversed-phase chromatography fractionation tailored to mass spectral characterization of humic substances. Environ Sci Technol. 2008;42(6):2060–5.CrossRefGoogle Scholar
  36. 36.
    Lv J, Zhang S, Luo L, Cao D. Solid-phase extraction-stepwise elution (SPE-SE) procedure for isolation of dissolved organic matter prior to ESI-FT-ICR-MS analysis. Anal Chim Acta. 2016;948:55–61.CrossRefGoogle Scholar
  37. 37.
    Ball GI, Aluwihare LI. CuO-oxidized dissolved organic matter (DOM) investigated with comprehensive two dimensional gas chromatography-time of flight-mass spectrometry (GC×GC-TOF-MS). Org Geochem. 2014;75:87–98.CrossRefGoogle Scholar
  38. 38.
    Benigni P, Thompson CJ, Ridgeway ME, Park MA, Fernandez-Lima F. Targeted high-resolution ion mobility separation coupled to ultrahigh-resolution mass spectrometry of endocrine disruptors in complex mixtures. Anal Chem. 2015;87(8):4321–5.CrossRefGoogle Scholar
  39. 39.
    Woods GC, Simpson MJ, Koerner PJ, Napoli A, Simpson AJ. HILIC-NMR: toward the identification of individual molecular components in dissolved organic matter. Environ Sci Technol. 2011;45(9):3880–6.  https://doi.org/10.1021/es103425s.CrossRefGoogle Scholar
  40. 40.
    Hockaday WC, Purcell JM, Marshall AG, Baldock JA, Hatcher PG. Electrospray and photoionization mass spectrometry for the characterization of organic matter in natural waters: a qualitative assessment. Limnol Oceanogr Methods. 2009;7(1):81–95.CrossRefGoogle Scholar
  41. 41.
    Jiao N, Zheng Q. The microbial carbon pump: from genes to ecosystems. Appl Environ Microbiol. 2011;77(21):7439–44.CrossRefGoogle Scholar
  42. 42.
    Jiao N, Herndl GJ, Hansell DA, Benner R, Kattner G, Wilhelm SW, et al. Microbial production of recalcitrant dissolved organic matter: long-term carbon storage in the global ocean. Nat Rev Microbiol. 2010;8:593–9.  https://doi.org/10.1038/nrmicro2386.CrossRefGoogle Scholar
  43. 43.
    Medeiros PM, Babcock-Adams L, Seidel M, Castelao RM, Iorio DD, Hollibaugh JT, et al. Export of terrigenous dissolved organic matter in a broad continental shelf. Limnol Oceanogr. 2017;62:1718–31.CrossRefGoogle Scholar
  44. 44.
    Seidel M, Yager PL, Ward ND, Carpenter EJ, Gomes HR, Krusche AV, et al. Molecular-level changes of dissolved organic matter along the Amazon River-to-ocean continuum. Mar Chem. 2015;177:218–31.CrossRefGoogle Scholar
  45. 45.
    Roth VN, Dittmar T, Gaupp R, Latitude GG. pH driven trends in the molecular composition of DOM across a north south transect along the Yenisei River. Geochim Cosmochim Acta. 2013;123(1):93–105.CrossRefGoogle Scholar

Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2019

Authors and Affiliations

  1. 1.State Key Laboratory of Heavy Oil ProcessingChina University of Petroleum (Beijing)BeijingChina

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