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Diffusion-ordered NMR spectroscopy (DOSY) is a powerful tool to analyse mixtures. Spatially encoded (SPEN) DOSY enables recording a full DOSY dataset in just one scan by performing spatial parallelisation of the gradient dimension. The simplest and most widely used approach to processing DOSY data is to fit each peak in the spectrum with a single or multiple exponential decay. However, when there is peak overlap, and/or when the diffusion decays of the contributing components are too similar, this method has limitations. Multivariate analysis of DOSY data, which is an attractive alternative, consists of decomposing the experimental data, into compound-specific diffusion decays and 1D NMR spectra. Multivariate analysis has been very successfully used for conventional DOSY data, but its use for SPEN DOSY data has only recently been reported. Here, we present a comparison, for SPEN DOSY data, of two widely used algorithms, SCORE and OUTSCORE, that aim at unmixing the spectra of overlapped species through a least square fit or a cross-talk minimisation, respectively. Data processing was performed with the General NMR Analysis Toolbox (GNAT), with custom-written code elements that now expands the capabilities, and makes it possible to import and process SPEN DOSY data. This comparison is demonstrated on three different two-component mixtures, each with different characteristics in terms of signal overlap, diffusion coefficient similarity, and component concentration.
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http://dx.doi.org/10.1002/mrc.5488 | DOI Listing |
Chem Sci
August 2025
Department of Chemistry, Michigan State University East Lansing USA
Exploration of the photophysical and photochemical properties of transition metal complexes has driven ground-breaking advancements in solar energy conversion technologies, including photoredox catalysis. While significant research has been devoted to understanding excited state properties of second- and third-row transition metal complexes, earth-abundant first-row metal complexes have received comparatively little attention in this context until very recently. In particular, the role of ion-pairing - which has been identified as a potentially significant factor for Ir(iii)-based photosensitizers - has not been examined with regard to its influence on the ligand-field excited states that dominate much of first-row photophysics.
View Article and Find Full Text PDFMagn Reson Chem
September 2025
Institut Català d'Investigació Química (ICIQ-CERCA), The Barcelona Institute of Science and Technology (BIST), Tarragona, Spain.
Multinuclear (H, P, and F) DOSY technique has been used under variable temperature conditions, in order to establish the optimal conditions for obtaining reliable data at variable temperatures, while keeping experimental settings as simple as possible (e.g., using standard NMR tubes).
View Article and Find Full Text PDFAnal Chim Acta
May 2025
Polymer and Biomaterials Chemistry Laboratory, Department of Chemistry and Biosciences, University of Bradford, Bradford, BD7 1DP, United Kingdom. Electronic address:
Question: This paper studies the importance of resolving 'in-solution' viscosity to determine an accurate hydrodynamic radii for high molar mass or high dispersity macromolecules via DOSY NMR. Analysis of polymer size via diffusion NMR has become increasingly more common, however as in-solution viscosity increases NMR output becomes more complex and requires dedicated methodologies (both in the instrumentation and data treatment) that can sufficiently resolve slowly diffusing analytes.
Results: Diffusion measurements were used to determine hydrodynamic radii of dissolved polymer chains of materials across a broad molar mass range in multiple solvents.
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 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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