Bacterial Cellulose Hybrid Composites with Calcium Phosphate for Bone Tissue Regeneration.

Bacterial cellulose (BC) is a unique microbial biopolymer with a huge number of significant applications in the biomedical field, including bone tissue engineering. The present study proposes to obtain and characterize BC hybrid composites with calcium phosphate as biocompatible and bioactive membranes for bone tissue engineering. BC precursor membranes were obtained in static culture fermentation, and after purification, were oxidized to obtain 2,3-dialdehyde bacterial cellulose (DABC). Calcium phosphate-BC oxidized membranes were produced by successive immersion in precursor solutions under ultrasonic irradiation. The samples were characterized for their physicochemical properties using scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy, attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy grazing incidence X-ray diffraction (GI-XRD), solid-state 13C nuclear magnetic resonance (CP/MAS 13C NMR), and complex thermal analysis. In vitro cell studies were also performed to evaluate the influence of modified morphological characteristics on cell adhesion and proliferation. The results showed an increase in porosity and biodegradability for DABC hybrid composites compared with BC. In vitro cell studies have revealed that both hybrid composites favor cell adhesion to the surface. The new BC and DABC hybrid composites with calcium phosphate could be considered promising materials for bone tissue regeneration.

Heteronuclear decoupling with rotor-synchronized phase-alternated cycles.

A new heteronuclear decoupling pulse sequence is introduced, dubbed ROtor-Synchronized Phase-Alternated Cycles (ROSPAC). It is based on a partial refocusing of the coherences (spin operator products or cross-terms) [Filip et al., J. Mag. Reson. 176, 2 (2005)] responsible for transverse spin-polarization dephasing, on the irradiation of a large pattern of radio-frequencies, and on a significant minimization of the cross-effects implying 1H chemical-shift anisotropy. Decoupling efficiency is analyzed by numerical simulations and experiments and compared to that of established decoupling sequences [swept-frequency two-pulse phase-modulated (TPPM), TPPM, small phase incremental alternation (SPINAL), refocused Continuous-wave (CWApa), and Rotor-Synchronized Hahn-Echo pulse train (RS-HEPT)]. It was found that ROSPAC offers good 1H offset robustness for a large range of chemical shifts and low radio-frequency (RF) powers, and performs very well in the ultra-fast magic-angle spinning (MAS) regime, where it is almost independent from RF power and permits it to avoid rotary-resonance recoupling conditions (v1 = nvr, n = 1, 2). It has the advantage that only the pulse lengths require optimization and has a low duty cycle in the pulsed decoupling regime. The efficiency of the decoupling sequence is demonstrated on a model microcrystalline sample of the model protein domain GB1 at 100 kHz MAS at 18.8 T.

Structural characterization of interfaces in silica core-alumina shell microspheres by solid-state NMR spectroscopy.

Atomic-scale description of surfaces and interfaces in core-shell aluminosilicate materials is not fully elucidated, partially due to their amorphous character and complex mechanisms that govern their properties. In this paper, new insights into nanostructured core-shell aluminosilicates have been demonstrated, by using different solid-state NMR methods, i.e 29Si, 29Si cross-polarization (CP), 27Al, 27Al triple-quantum (3Q), and 1H-27Al heteronuclear correlation (HETCOR) MAS NMR. For this purpose, nanostructured silica core-alumina shell microspheres, undoped and doped with gadolinium ions respectively, obtained by a chemical synthesis based on the Stöber method for the silica core and electrostatic attraction for developing the alumina shell were studied. As a result, a new alumino-silicate layer formation was proved at the interface between silica core, where aluminum diffuses, on small scale, in the silica network, and alumina shell, where silicon ions migrate, on a larger scale, in the alumina network, leading to a stable core-shell structure. Moreover, this process is accompanied by significant local structural changes in the transition zone, particularly at the aluminum neighborhood, which is quite well understood now, with the power of solid-state NMR spectroscopy.

Conformational Preference and Spectroscopical Characteristics of the Active Pharmaceutical Ingredient Levetiracetam.

The analysis of the possible conformers and the conformational change between solid and liquid states of a particular drug molecule are mandatory not only for describing reliably its spectroscopical properties but also for understanding the interaction with the receptor and its mechanism of action. Therefore, here we investigated the free-energy conformational landscape of levetiracetam (LEV) in gas phase as well as in water and ethanol, aiming to describe the 3-dimensional structure and energetic stability of its conformers. Twenty-two unique conformers were identified, and their energetic stability was determined at density functional theory B3LYP/6-31+G(2d,2p) level of theory. The 6 most stable monomers in water, within a relative free-energy window of 0.71 kcal mol-1 and clearly separated in energy from the remaining subset of 16 conformers, as well as the 3 most stable dimers were then used to compute the Boltzmann populations-averaged UV-Vis and NMR spectra of LEV. The conformational landscape in solution is distinctly different from that corresponding to gas phase, particularly due to the relative orientations of the butanamide group. Aiming to clarify the stability of the possible dimers of LEV, we also investigated computationally the structure of a set of 11 nonhydrated and hydrated homochiral hydrogen-bonded LEV dimers.

Preparation, characterization, and testing of metal-doped carbon xerogels as catalyst for phenol CWAO.

Co-, Ce-, and Ni-doped carbon xerogels (Me-CX) synthesized by sol-gel method followed by an ion exchange process were used as catalysts for catalytic wet air oxidation (CWAO) of phenol. The prepared catalysts were characterized using TEM, SEM, BET surface area, and XRD. Me-CX catalysts were tested in mild conditions (20-60 °C, atmospheric pressure) in a semi-batch reactor in various reaction conditions (30-60 L/h, 0.05-0.2 g catalysts, 50-175 mg phenol/L). Total organic carbon (TOC) removal efficiency values obtained decrease in the following order Co-CX â‰… Ce-CX > Ni1-CX > K-CX for the catalysts obtained using the same procedure. TOC removal efficiencies of up to 72% were reached in case of Co-CX catalyst at 20 °C, 40 L/h, using 0.15 g catalyst and a solution of 100 mg phenol/L.

Physically and chemically cross-linked cellulose cryogels: Structure, properties and application for controlled release.

Porous cellulose matrices were prepared via cellulose dissolution in 8wt% NaOH-water, physical gelation and chemical cross-linking with epichlorohydrin (ECH), coagulation in water and lyophilisation. Cellulose and cross-linker concentration were varied. The behaviour of gels upon coagulation and the swelling of cryogels in water were analysed. An anomalous high swelling at cross-linker concentration around stoichiometric molar ratio with cellulose was observed. Cellulose cryogel morphology, crystallinity and density were studied. The influence of chemical cross-linking on cellulose swelling was explained by suggesting that ECH acts as a spacer preventing cellulose chains tight packing during coagulation. Cellulose was loaded with a model drug, procaine hydrochloride, and the kinetics of its release was investigated.

Heterocycles 27. Microwave assisted synthesis and antitumour activity of novel phenothiazinyl-thiazolyl-hydrazine derivatives.

A series of new phenothiazinyl-thiazolyl-hydrazine derivatives were synthesized by Hantzsch cyclization of 1-(10-ethyl-10H-phenothiazin-3-yl)-methylidene-thiosemicarbazide with α-halocarbonyl derivatives. Comparison between classical and microwave assisted synthesis emphasizes the great advantages induced by microwaves irradiation which afforded high reaction yields in much shorter reaction time. Structural assignments were based on spectroscopic methods (high resolution NMR, FTIR, MS). The new compounds were tested in vitro for their antiproliferative activity against tumor cell lines using spectrometric methods. Most of the compounds exhibit cytotoxicity against hepatic and colon tumor cells in a dose-dependent mode and a relationship between the structure and their biological activity was observed.