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

被引：11

作者：

Pages, Guilhem ^{[1
,2
]}

Bonny, Alice ^{[1
]}

Gilard, Veronique ^{[1
]}

Malet-Martino, Myriam ^{[1
]}

机构：

[1] Univ Toulouse, Grp RMN Biomed, Lab Synth & Phys Chim Mol Interet Biol, UMR CNRS 5068, 118 Route Narbonne, F-31062 Toulouse 9, France

[2] INRA, Qual Prod Anim UR370, F-63122 St Genes Champanelle, France

来源：

ANALYTICAL CHEMISTRY | 2016年 / 88卷 / 06期

关键词：

LEAST-SQUARES ANALYSIS; SPECTRAL DATA SETS; 2D DOSY H-1-NMR; RESOLUTION; ALGORITHM; TOOL; DIFFUSOMETRY; DIFFRACTION; DIMENSIONS; KINETICS;

D O I：

10.1021/acs.analchem.5b04781

中图分类号：

O65 [分析化学];

学科分类号：

070302 ; 081704 ;

摘要：

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.

引用

页码：3304 / 3309

页数：6