Residual Dipolar Coupling to Quadrupolar Nuclei with Negative Gyromagnetic Ratios in MAS NMR. Implications for (29Si,14N) Effects in29Si Solid-State NMR Spectra

Author(s):  
Alejandro C. Olivieri
2016 ◽  
Vol 18 (36) ◽  
pp. 25284-25295 ◽  
Author(s):  
Aaron J. Rossini ◽  
Michael P. Hanrahan ◽  
Martin Thuo

Fast MAS and proton detection are applied to rapidly acquire wideline solid-state NMR spectra of spin-1/2 and half-integer quadrupolar nuclei.


2017 ◽  
Vol 13 ◽  
pp. 182-194 ◽  
Author(s):  
Monica Ferro ◽  
Franca Castiglione ◽  
Nadia Pastori ◽  
Carlo Punta ◽  
Lucio Melone ◽  
...  

Two different formulations of cyclodextrin nanosponges (CDNS), obtained by polycondensation of β-cyclodextrin with ethylenediaminetetraacetic acid dianhydride (EDTAn), were treated with aqueous solutions of ibuprofen sodium salt (IbuNa) affording hydrogels that, after lyophilisation, gave two solid CDNS-drug formulations. 1H fast MAS NMR and 13C CP-MAS NMR spectra showed that IbuNa was converted in situ into its acidic and dimeric form (IbuH) after freeze-drying. 13C CP-MAS NMR spectra also indicated that the structure of the nanosponge did not undergo changes upon drug loading compared to the unloaded system. However, the 13C NMR spectra collected under variable contact time cross-polarization (VCT-CP) conditions showed that the polymeric scaffold CDNS changed significantly its dynamic regime on passing from the empty CDNS to the drug-loaded CDNS, thus showing that the drug encapsulation can be seen as the formation of a real supramolecular aggregate rather than a conglomerate of two solid components. Finally, the structural features obtained from the different solid-state NMR approaches reported matched the information from powder X-ray diffraction profiles.


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