Diffusion-ordered NMR spectroscopy (DOSY) presents an essential tool for the analysis of compound mixtures by revealing intrinsic diffusion behaviors of mixed components. The applicability of DOSY measurements on complex mixtures is generally limited by the performance of data reconstruction algorithms. Here, based on constraints on low rank and sparsity of DOSY data, we propose a reconstruction method to achieve high-resolution DOSY spectra with excellent peak alignments and accurate diffusion coefficients for measurements of complex mixtures even when component signals are congested and mixed together along the spectral dimension. This proposed method is robust and suitable for DOSY data acquired from common commercial NMR instruments; thus, it may broaden the scope of DOSY applications.
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http://dx.doi.org/10.1021/acs.analchem.9b03865 | DOI Listing |
Anal Chem
December 2024
Department of Chemistry, University of Manchester, Oxford Road, Manchester M13 9PL, United Kingdom.
Mixture analysis is crucial in many areas of chemistry, and a wide variety of separation methods are in use. A common method for physical separation is high-performance liquid chromatography (HPLC), but resolution is a problem: chemically similar species coelute. An alternative approach is diffusion-ordered NMR spectroscopy (DOSY), in which the signals of mixture components are separated according to the diffusion coefficient.
View Article and Find Full Text PDFChemistry
December 2024
Hiroshima University, Chemistry, 1-3-1 Kagamiyama, 739-8526, Higashi-Hiroshima, JAPAN.
The intermolecular host-guest complexation of head-to-tail monomers consisting of cleft-shaped bisporphyrin and trinitrofluorenone units connected by a chiral binaphthyl linker was employed to construct helically twisted supramolecular polymers. Results from 1H NMR, diffusion-ordered NMR spectroscopy, and viscometry experiments revealed that the supramolecular polymerization of these monomers follows a ring-chain competition mechanism. The introduction of bulky substituents at the linker significantly suppressed the formation of macrocyclic oligomers, whereas smaller alkyl chains facilitated the formation of the cyclic form.
View Article and Find Full Text PDFMagn Reson Chem
December 2024
Department of Chemistry, NMR Centre, Laboratory of Analytical Chemistry, University of Ioannina, Ioannina, Greece.
New psychoactive substances (NPS)-designed to mimic various legal or illegal substances-are an emerging worldwide health problem. Their identification and quantification in either complex seized samples or powders are critical; moreover, their determination in biological fluids is an intriguing goal in the forensic toxicology field. Synthetic cathinones are one of the most important groups among NPS.
View Article and Find Full Text PDFCarbohydr Polym
February 2025
Department of Pharmacy, University of Oslo, P.O. Box 1068 Blindern, NO-136 Oslo, Norway. Electronic address:
The potential of DOSY NMR spectroscopy to distinguish the linkage pattern of chemically related polysaccharides was evaluated using β-glucans isolated from yeast (Saccharomyces cerevisiae) and mushroom (Pleurotus eryngii). Laminarin from Laminaria digitata was included for chemical shift comparison. Characterization through methylation and 1D/2D NMR analysis showed that all the samples were constituted by →3)-Glcp-(1→; →3,6)-Glcp-(1→; Glcp-(1→ and →6)-Glcp-(1→ linkages.
View Article and Find Full Text PDFLangmuir
December 2024
Department of Pharmaceutics, National Institute of Pharmaceutical Education and Research (NIPER)-Raebareli, Lucknow 226002, India.
Block copolymer micelles have been increasingly used for the solubilization and delivery of hydrophobic drugs. There exists a possibility of dissociation of micelles and formation of other association structures in contact with the gastrointestinal fluid. In this study, we demonstrated the effect of the fed-state intestinal fluid (FeSSIF) upon characteristics of bare and quercetin (QCT)-loaded pluronic 123 (P123) micelles.
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