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Diffusion-ordered spectroscopy on a benchtop spectrometer for drug analysis.

Gaëtan Assemat1, Boris Gouilleux2, Dylan Bouillaud2

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|August 15, 2018
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Summary
This summary is machine-generated.

This study introduces low-field (LF) two-dimensional diffusion-ordered spectroscopy (DOSY) for pharmaceutical analysis. LF DOSY successfully separates components in formulations and medicines, offering a valuable tool for complex mixture analysis.

Keywords:
Benchtop NMRDOSY NMRDrug analysisLow field NMR

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Area of Science:

  • Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Analytical Chemistry
  • Pharmaceutical Analysis

Background:

  • Two-dimensional diffusion-ordered spectroscopy (2D DOSY) is a powerful NMR technique for analyzing complex mixtures.
  • Low-field (LF) NMR offers advantages in terms of cost and accessibility, but its application in DOSY has been limited.
  • Developing robust LF DOSY methods is crucial for broader adoption in pharmaceutical research.

Purpose of the Study:

  • To report the first two-dimensional diffusion-ordered spectroscopy (DOSY) experiments conducted at low field (LF).
  • To evaluate the efficacy of LF DOSY for analyzing pharmaceutical formulations and medicines.
  • To compare different gradient sampling schemes for optimizing LF DOSY experiments.

Main Methods:

  • Utilized a benchtop NMR spectrometer for LF DOSY experiments.
  • Employed the bipolar pulse pair-stimulated echo sequence with a longitudinal eddy current delay (BPP-STE-LED) pulse sequence.
  • Applied LF DOSY to a model pharmaceutical formulation and a real esomeprazole medicine, comparing linear, exponential, and semi-Gaussian (SG) gradient schemes.

Main Results:

  • Achieved clear separation of components in a model pharmaceutical formulation using LF DOSY.
  • Obtained apparent diffusion coefficient (ADC) values consistent with high-field NMR measurements.
  • Identified the semi-Gaussian (SG) ramp as the most reliable gradient sampling scheme for LF DOSY.
  • Demonstrated the utility of the diffusion dimension for assigning overcrowded LF spectra, despite challenges with highly overlapped signals.

Conclusions:

  • LF DOSY is a viable technique for analyzing pharmaceutical mixtures on a benchtop NMR spectrometer.
  • The diffusion dimension in LF DOSY is highly beneficial for spectral assignment in complex samples.
  • Further optimization is needed to obtain accurate ADC values for all components in highly overlapped spectra.