The main objective of the current study was to investigate penetration of cell penetrating peptides (CPPs: TAT, R8, R11, and YKA) through skin intercellular lipids using (31)P magic angle spinning (MAS) solid-state NMR. In vitro skin permeation studies were performed on rat skin, and sections (0-60, 61-120, and 121-180μm) were collected and analyzed for (31)P NMR signal. The concentration-dependent shift of 0, 25, 50, 100, and 200mg/ml of TAT on skin layers, diffusion of TAT, R8, R11, and YKA in the skin and time dependent permeation of R11 was measured on various skin sections using (31)P solid-state NMR. Further, CPPs and CPP-tagged fluorescent dye encapsulate liposomes (FLip) in skin layers were tagged using confocal microscopy. The change in (31)P NMR chemical shift was found to depend monotonically on the amount of CPP applied on skin, with saturation behavior above 100mg/ml CPP concentration. R11 and TAT caused more shift in solid-state NMR peaks compared to other peptides. Furthermore, NMR spectra showed R11 penetration up to 180μm within 30min. The results of the solid-state NMR study were in agreement with confocal microscopy studies. Thus, (31)P solid-state NMR can be used to track CPP penetration into different skin layers.
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http://dx.doi.org/10.1016/j.ejpb.2013.05.003 | DOI Listing |
Chem Sci
December 2024
State Key Laboratory of Catalysis, Dalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics, Chinese Academy of Sciences Zhongshan Road 457 Dalian 116023 China
In solid-state NMR, dipolar-based heteronuclear polarization transfer has been extensively used for sensitivity enhancement and multidimensional correlations, but its efficiency often suffers from undesired spin interactions and hardware limitations. Herein, we propose a novel dipolar-echo edited R-symmetry (DEER) sequence, which is further incorporated into the INEPT-type scheme, dubbed DEER-INEPT, for achieving highly efficient heteronuclear polarization transfer. Numerical simulations and NMR experiments demonstrate that DEER-INEPT offers significantly improved robustness, enabling efficient polarization transfer under a wide range of MAS conditions, from slow to ultrafast rates, outperforming existing methods.
View Article and Find Full Text PDFInt J Biol Macromol
January 2025
College of Chemistry and Chemical Engineering, Southwest Petroleum University, Chengdu 610500, PR China; Engineering Research Center of Oilfield Chemistry, Ministry of Education, Chengdu 610500, PR China; Oil & Gas Field Applied Chemistry Key Laboratory of Sichuan Province, Chengdu 610500, PR China. Electronic address:
In this study, polyamide/silica/sodium alginate (SA) composite (PA-Si-SA) was successfully prepared in one-step benzoxazine-isocyanide chemistry (BIC)/sol-gel process at room temperature. The chemical structure and fundamental properties of PA-Si-SA were characterized by FT-IR, solid-state C NMR, XPS, XRD, SEM, BET and TG, etc. The presence of anionic SA and diverse N, O-containing functional segments (amide, tertiary amine, alkyl/phenol -OH, Si-O-Si, and COO) in PA-Si-SA endows it synergistic complexation capability toward Pb and Cd.
View Article and Find Full Text PDFInorg Chem
January 2025
Department of Chemistry, Western Michigan University, Kalamazoo, Michigan 49008, United States.
The supramolecular binding exclusively by H-bonds of SeO, MoO and WO ions to form nanojars of the formula [EO⊂{-Cu(μ-OH)(μ-pz)}] (; E = Se, Mo, W; = 28-34; pz = pyrazolate) was studied in solution by electrospray ionization mass spectrometry, variable temperature, paramagnetic H NMR and UV-vis spectroscopy, and in the solid state by single-crystal X-ray crystallography. These large anions allow for the observation of a record nanojar size, (E = Mo, W). Six crystal structures are described of nanojars of varying sizes with either SeO, MoO or WO entrapped ions, including the first example of a cocrystal of two different nanojars in crystallographically unique positions, and .
View Article and Find Full Text PDFIUCrJ
January 2025
Centre of Molecular and Macromolecular Studies, Polish Academy of Sciences, Sienkiewicza 112, Lodz 90-363, Poland.
Crystal structure determination is a crucial aspect of almost every branch of the chemical sciences, bringing us closer to understanding crystallization, polymorphism, phase transitions, and the relationship between a structure and its physicochemical and functional properties. Unfortunately, many molecules notoriously crystallize as microcrystalline powders, providing a significant challenge in establishing their structures. In this work, we describe the crystal structure determination of three elusive polymorphs of the anti-inflammatory drug meloxicam (MLX) using three approaches, of which only one was successful for each crystal phase.
View Article and Find Full Text PDFSci Rep
January 2025
Ali I. Al-Naimi Petroleum Engineering Research Center, King Abdullah University of Science and Technology, Thuwal, Saudi Arabia.
Microbial impacts on early carbonate diagenesis, particularly the formation of Mg-carbonates at low temperatures, have long eluded scientists. Our breakthrough laboratory experiments with two species of halophilic aerobic bacteria and marine carbonate grains reveal that these bacteria created a distinctive protodolomite (disordered dolomite) rim around the grains. Scanning Electron Microscopy (SEM) and X-ray Diffraction (XRD) confirmed the protodolomite formation, while solid-state nuclear magnetic resonance (NMR) revealed bacterial interactions with carboxylated organic matter, such as extracellular polymeric substances (EPS).
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