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13C quantification in heterogeneous multiphase natural samples by CMP-NMR using stepped decoupling.

Paris Ning1, Ronald Soong1, Wolfgang Bermel2

  • 1Environmental NMR Centre, University of Toronto Scarborough, 1265 Military Trail, Toronto, ON, M1C 1A4, Canada.

Analytical and Bioanalytical Chemistry
|August 15, 2018
PubMed
Summary
This summary is machine-generated.

This study introduces comprehensive multiphase nuclear magnetic resonance (CMP-NMR) for analyzing intact samples. The new stepped decoupling method enables accurate quantification of liquids, gels, and solids in natural samples.

Keywords:
CMP-NMRDecouplingMultiphase NMRMultiphase quantificationNatural intact samples

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Area of Science:

  • Analytical Chemistry
  • Spectroscopy
  • Biophysical Chemistry

Background:

  • Natural and environmental samples often contain complex mixtures of liquids, gels, and solids.
  • Quantifying components across multiple phases in intact samples without pre-treatment is a significant analytical challenge.
  • Existing methods like high-resolution magic angle spinning (HR-MAS) have limitations in handling all sample phases simultaneously.

Purpose of the Study:

  • To develop and validate a method for accurate quantification of all components within intact multiphase samples using nuclear magnetic resonance (NMR).
  • To address the challenges of analyzing complex mixtures containing liquids, gels, and solids in their native state.
  • To enable the detection and quantification of both major chemical categories and individual species, including volatile compounds.

Main Methods:

  • Introduction of Comprehensive Multiphase Nuclear Magnetic Resonance (CMP-NMR) by integrating HR-MAS capabilities with full solids power handling.
  • Development and application of a novel 'stepped decoupling' pulse sequence for effective 1H decoupling across all sample phases (liquid, gel, solid).
  • Utilizing 13C NMR for quantification due to less broadening in the solid-state compared to 1H NMR, coupled with optimized decoupling conditions.

Main Results:

  • The stepped decoupling sequence provides high-resolution spectra without truncation artifacts, enabling accurate quantification of components in all phases.
  • Demonstrated accurate quantification of chemical categories (e.g., total carbohydrates) and individual species (e.g., glucose) in standards and natural samples (broccoli, soil, Arabidopsis).
  • Successfully quantified volatile species like methanol and ethylene in intact Arabidopsis samples, which are typically difficult to detect.

Conclusions:

  • CMP-NMR with stepped decoupling offers a robust solution for analyzing intact multiphase samples, overcoming previous limitations in quantification.
  • The method allows for comprehensive chemical profiling of complex natural and environmental samples without destructive pre-treatment.
  • This technique significantly advances the ability to study chemical composition and volatile emissions from biological and environmental matrices.