Sequential extraction protocol for organic matter from soils and sediments using high resolution mass spectrometry

Malak M. Tfaily, Rosalie K. Chu, Jason Toyoda, Nikola Tolić, Errol W. Robinson, Ljiljana Paša-Tolić, Nancy J. Hess

Research output: Contribution to journalArticlepeer-review

95 Scopus citations


A vast number of organic compounds are present in soil organic matter (SOM) and play an important role in the terrestrial carbon cycle, facilitate interactions between organisms, and represent a sink for atmospheric CO2. The diversity of different SOM compounds and their molecular characteristics is a function of the organic source material and biogeochemical history. By understanding how SOM composition changes with sources and the processes by which it is biogeochemically altered in different terrestrial ecosystems, it may be possible to predict nutrient and carbon cycling, response to system perturbations, and impact of climate change will have on SOM composition. In this study, a sequential chemical extraction procedure was developed to reveal the diversity of organic matter (OM) in different ecosystems and was compared to the previously published protocol using parallel solvent extraction (PSE). We compared six extraction methods using three sample types, peat soil, spruce forest soil and river sediment, so as to select the best method for extracting a representative fraction of organic matter from soils and sediments from a wide range of ecosystems. We estimated the extraction yield of dissolved organic carbon (DOC) by total organic carbon analysis, and measured the composition of extracted OM using high resolution mass spectrometry. This study showed that OM composition depends primarily on soil and sediment characteristics. Two sequential extraction protocols, progressing from polar to non-polar solvents, were found to provide the highest number and diversity of organic compounds extracted from the soil and sediments. Water (H2O) is the first solvent used for both protocols followed by either co-extraction with methanol-chloroform (MeOH-CHCl3) mixture, or acetonitrile (ACN) and CHCl3 sequentially. The sequential extraction protocol developed in this study offers improved sensitivity, and requires less sample compared to the PSE workflow where a new sample is used for each solvent type. Furthermore, a comparison of SOM composition from the different sample types revealed that our sequential protocol allows for ecosystem comparisons based on the diversity of compounds present, which in turn could provide new insights about source and processing of organic compounds in different soil and sediment types.

Original languageEnglish (US)
Pages (from-to)54-61
Number of pages8
JournalAnalytica Chimica Acta
StatePublished - Jun 15 2017
Externally publishedYes


  • Carbon cycle
  • Charge competition
  • Ionization efficiency
  • Mass spectrometry
  • Sediments
  • Soil organic matter

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry
  • Environmental Chemistry
  • Spectroscopy


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