Pulsed Field Gradient NMR with Sigmoid Shape Gradient Sampling To Produce More Detailed Diffusion Ordered Spectroscopy Maps of Real Complex Mixtures: Examples with Medicine Analysis

Pulsed Field Gradient NMR with Sigmoid Shape Gradient Sampling To Produce More Detailed Diffusion Ordered Spectroscopy Maps of Real Complex Mixtures: Examples with Medicine Analysis

NMR diffusion measurements are based on signal attenuation. In the case of complex mixtures for which some molecules are diffusing quickly while others are significantly slower, it is challenging to obtain a diffusion ordered spectroscopy (DOSY)-type 2D map giving reliable information on all molecul...

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Bibliographic Details
Published in:Analytical chemistry (Washington) Vol. 88; no. 6; pp. 3304 - 3309
Main Authors: Pagès, Guilhem, Bonny, Alice, Gilard, Véronique, Malet-Martino, Myriam
Format: Journal Article
Language:English
Published: United States American Chemical Society 15-03-2016
Subjects:
Analytical chemistry
Chemical Sciences
Complex Mixtures
Diffusion
Diffusion rate
Magnetic Resonance Spectroscopy - methods
Medicine
Molecules
NMR
Nuclear magnetic resonance
Ramps
Sampling
Spectroscopy
Spectrum Analysis - methods
Strategy
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Summary:NMR diffusion measurements are based on signal attenuation. In the case of complex mixtures for which some molecules are diffusing quickly while others are significantly slower, it is challenging to obtain a diffusion ordered spectroscopy (DOSY)-type 2D map giving reliable information on all molecules. In this paper, we propose a new gradient sampling approach based on a sigmoid shape allowing the acquisition of a significant number of points for both the fast and slow diffusing molecules. We applied this new gradient sampling strategy to deformulate two medicines whose composition was known (Esomeprazole) or unknown (Mebendazole). PFG NMR associated with a sigmoid gradient ramp is an exciting strategy to study drugs as a whole, i.e., the active ingredient(s) and excipients.
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ISSN:0003-2700
1520-6882
DOI:10.1021/acs.analchem.5b04781