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Size-exclusion chromatographic NMR under HR-MAS

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journal contribution
posted on 2023-06-09, 01:45 authored by Guillermo Lucena Alcalde, Natalie Anderson, Iain Day
The addition of stationary phases or sample modifiers can be used to modify the separation achievable in the diffusion domain of diffusion NMR experiments or provide information on the nature of the analyte–sample modifier interaction. Unfortunately, the addition of insoluble chromatographic stationary phases can lead to line broadening and degradation in spectral resolution, largely because of differences in magnetic susceptibility between the sample and the stationary phase. High-resolution magic angle spinning (HR-MAS) techniques can be used to remove this broadening. Here, we attempt the application of HR-MAS to size-exclusion chromatographic NMR with limited success. Observed diffusion coefficients for polymer molecular weight reference standards are shown to be larger than those obtained on static samples. Further investigation reveals that under HR-MAS it is possible to obtain reasonably accurate estimates of diffusion coefficients, using either full rotor synchronisation or sophisticated pulse sequences. The requirement for restricting the sample to the centre of the MAS rotor to ensure homogeneous magnetic and RF fields is also tested.

Funding

NMR Studies of the Early Stages of Aggregation Phenomena; G0186; EPSRC-ENGINEERING & PHYSICAL SCIENCES RESEARCH COUNCIL; EP/H025367/1

History

Publication status

  • Published

File Version

  • Accepted version

Journal

Magnetic Resonance in Chemistry

ISSN

0749-1581

Publisher

Wiley

Issue

5

Volume

55

Page range

485-491

Department affiliated with

  • Chemistry Publications

Full text available

  • Yes

Peer reviewed?

  • Yes

Legacy Posted Date

2016-06-20

First Open Access (FOA) Date

2017-06-16

First Compliant Deposit (FCD) Date

2016-06-20

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