Journal Article FZJ-2017-07699

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Diffusion-Ordered Nuclear Magnetic Resonance Spectroscopy (DOSY-NMR): A Novel Tool for Identification of Phosphorus Compounds in Soil Extracts

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2017
American Chemical Society Columbus, Ohio

Environmental science & technology 51(22), 13256 - 13264 () [10.1021/acs.est.7b03322]

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Abstract: Liquid-state, one-dimension 31P nuclear magnetic resonance spectroscopy (NMR) has greatly advanced our understanding of the composition of organic phosphorus in the environment. However, the correct assignment of signals is complicated by overlapping and shifting signals in different types of soils. We applied therefore for the first time diffusion-ordered spectroscopy (DOSY) to soil extracts, allowing us to separate phosphorus components in the second domain based on their translational diffusion coefficients. After successful application to a mixture of 14 model compounds, diffusion rates correlated closely with the molecular weight of the individual compound in aqueous solution (R2 = 0.97). The method was then applied to NaOH/EDTA extracts of a grassland soil, of which paramagnetic contaminations were removed with sodium sulfide following high-velocity centrifugation (21 500g, 45 min) at 4 °C. Diffusion rates in soil extracts were again closely related to molecular weight (R2 = 0.98), varying from 163.9 to 923.8 Da. However, our DOSY application failed for a forest soil with low organic phosphorus content. Overall, DOSY did help to clearly identify specific NMR signals like myo- and scyllo-inositol hexakisphosphate. It thus provides a more confident signal assignment than 1D 31P NMR, although currently the ubiquitous use of this novel methodology is still limited to soils with high organic phosphorus content.

Classification:

Contributing Institute(s):
  1. Analytik (ZEA-3)
  2. Agrosphäre (IBG-3)
Research Program(s):
  1. 255 - Terrestrial Systems: From Observation to Prediction (POF3-255) (POF3-255)
  2. HITEC - Helmholtz Interdisciplinary Doctoral Training in Energy and Climate Research (HITEC) (HITEC-20170406) (HITEC-20170406)

Appears in the scientific report 2017
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 Record created 2017-11-23, last modified 2021-01-29


Published on 2017-10-25. Available in OpenAccess from 2018-10-25.:
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