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- Acid-modified clays as green catalysts for the hydrolysis of hemicellulosic oligosaccharidesPublication . Vilcocq, Léa; Spínola, Vítor; Moniz, Patrícia; Duarte, Luís C.; Carvalheiro, Florbela; Fernandes, César; Castilho, PaulaThe hydrolysis of hemicellulosic oligosaccharides (OS) was investigated using acid-activated clays (prepared from natural Porto Santo montmorillonite clay) as catalysts. Acid activation was performed in HCl solution or with aluminium exchange. The clay catalysts were characterized by XRD, N2 adsorption isotherms, CEC, FTIR, titration of acid sites in water and adsorption of sugars and disaccharides. They were tested for the hydrolysis of a model compound, maltose, and of OS-rich liquor from rice straw fractionation. The HCl-activated clays were the most efficient catalysts for maltose hydrolysis. It was demonstrated that the hydrolysis of OS into monomer sugars over a clay catalyst is technically feasible and that this reaction leads to the selective removal of glucose, arabinose and acetic acid side groups from the OS structure, thus yielding simpler xylo-oligosaccharide chains. Furthermore, no significant conversion of monomer sugars into furans was observed.
- Influence of exchange cations on the catalytic conversion of limonene over Serra de Dentro (SD) and SAz-1 clays: correlations between acidity and catalytic activity/selectivityPublication . Catrinescu, C.; Fernandes, César; Castilho, P.; Breen, C.A bentonite collected at Serra de Dentro (SD), Porto Santo Island, Portugal, and the source clay SAz-1 (Cheto, Arizona) were ion-exchanged with different cations (Al3+, Ni2+, Cr3+ and Na+ ). Variable temperature diffuse reflectance infrared Fourier transform spectroscopy (VT-DRIFTS) of pyridine treated samples, thermal desorption of cyclohexylamine and real time mass spectrometry of the evolved gases were used to evaluate the acidic properties of the prepared catalysts. The catalytic activity of these ion-exchanged clays was tested in the acid-catalysed conversion of limonene at 150 8C, to yield isomerization products (terpinolene, a-terpinene, g-terpinene and isoterpinolene), disproportionation products ( p cymene and p-menthenes) and high molecular-weight compounds. The possibility of increasing the selectivity toward p-cymene, over a catalyst with substantial Lewis acid character, was particularly envisaged. Catalysts derived from SD were significantly more active than their SAz-1 counterparts. This was mainly attributed to the greater inherent acidity, to the higher structural iron content (providing dehydrogenation activity) and to the higher nitrogen surface area of the starting SD clays. Within the Mn+ -SD series, the order of activity decreased as Ni2+ > Al3+ > Cr3+ > Na+ . A direct comparison between Al3+-SD (with maximized Bro¨nsted acidity) and Ni2+-SD (with predominant Lewis acid character) provided no support for enhanced p-cymene production over Lewis acid sites.
- Calcium phosphate-mediated gene delivery using simulated body fluid (SBF)Publication . Nouri, Alireza; Castro, Rita; Santos, José L.; Fernandes, César; Rodrigues, João; Tomás, HelenaThe present study aimed at developing a new approach in gene delivery of calcium phosphate nanoparticles through simulated body fluid (CaP-SBF). The physicochemical and biological characteristics of the CaP-SBF nanoparticles were compared with those made in pure water (CaP-water) via a similar procedure. The CaP-SBF and CaP-water solutions were then adjusted to two different pH values of 7.4 and 8.0, mixed with plasmid DNA (pDNA), and added in varying amounts to human embryonic kidney (HEK 293T) cells. The transfection efficiency and cell viability were studied in vitro by reporter gene (luciferase and Enhanced Green Fluorescent Protein) expression and the resazurin reduction assay, respectively, 24 and 48 h after the incubation with the nanoparticles. Our results indicated considerably high in vitro transfection efficiency for CaP-SBF/DNA complexes at physiological pH (7.4) with high amounts of CaP. Additionally, the SBF solution exhibited the ability to reduce the rapid growth of CaP particles over time, leading to higher transfection efficiency of CaP-SBF/DNA complexes than those made in water (CaP-water/DNA).