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Dias, D, Lapa N, Bernardo M, Godinho D, Fonseca I, Miranda M, Pinto F, Lemos F.  2017.  Properties of chars from the gasification and pyrolysis of rice waste streams towards their valorisation as adsorbent materials. Waste Management. 65:186-194. AbstractWebsite

Rice straw (RS), rice husk (RH) and polyethylene (PE) were blended and submitted to gasification and pyrolysis processes. The chars obtained were submitted to textural, chemical, and ecotoxic characterisations, towards their possible valorisation. Gasification chars were mainly composed of ashes (73.4–89.8wt%), while pyrolysis chars were mainly composed of carbon (53.0–57.6wt%). Silicon (Si) was the major mineral element in all chars followed by alkaline and alkaline-earth metal species (AAEMs). In the pyrolysis chars, titanium (Ti) was also a major element, as the feedstock blends contained high fractions of PE which was the main source of Ti. Gasification chars showed higher surface areas (26.9–62.9m2g−1) and some microporosity, attributed to porous silica. On the contrary, pyrolysis chars did not present a porous matrix, mainly due to their high volatile matter content. The gasification bed char produced with 100% RH, at 850°C, with O2 as gasification agent, was selected for further characterization. This char presented the higher potential to be valorised as adsorbent material (higher surface area, higher content of metal cations with exchangeable capacity, and lowest concentrations of toxic heavy metals). The char was submitted to an aqueous leaching test to assess the mobility of chemical species and the ecotoxic level for V. fischeri. It was observed that metallic elements were significantly retained in the char, which was attributed mainly to its alkaline character. This alkaline condition promoted some ecotoxicity level on the char eluate that was eliminated after the pH correction.

Agostinho, DAS, Paninho AI, Cordeiro T, Nunes AVM, Fonseca IM, Pereira C, Matias A, Ventura MG.  2020.  Properties of κ-carrageenan aerogels prepared by using different dissolution media and its application as drug delivery systems. Materials Chemistry and Physics. 253:123290. AbstractWebsite

This work reports the synthesis of kappa-carrageenan aerogels using different dissolution and crosslinking media in order to evaluate its effects on the textural properties of the matrixes and further on the drug loading and release performance. The different aerogel samples were produced through the dissolution of the biopolymer in water with addition of potassium salts as crosslinking agents and, in two different ionic liquids (ILs) derived from imidazolium ion, being further dried with supercritical CO2. The samples were characterized by Attenuated Total Reflectance-Fourier Transform Infrared Spectroscopy (ATR-FTIR), Scanning Electron Microscopy (SEM), Nitrogen Adsorption-Desorption Analysis, Thermogravimetry (TGA) and Differential Scanning Calorimetry (DSC). The synthesized samples presented surface areas similar to the carrageenan aerogels being their structure constituted mainly by meso and macropores. The absence of ionic liquid in samples was demonstrated by DSC analysis and was corroborated by the cytotoxicity assays which revealed that cellular viability in Caco-2 cells was preserved. Tetracycline was used as a model drug and loaded in two of the prepared aerogels samples. The release experiments were performed with the composites to test in vitro drug release at physiologic pH. With a higher macroporosity, the kappa-carrageenan aerogel prepared by dissolution into ionic liquid showed a higher loading capacity than the one prepared by dissolution into water and a slightly higher release rate. The matrixes were considered to present a good potential to be used as biocompatible carriers on drug controlled delivery.

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Madureira, J, Melo R, Verde SC, Matos I, Bernardo M, Noronha JP, Marga{\c c}a FMA, Fonseca IM.  2018.  Recovery of phenolic compounds from multi-component solution by a synthesized activated carbon using resorcinol and formaldehyde. Water Science and Technology. 77:456–466., Number 2: IWA Publishing AbstractWebsite

The adsorption of four phenolic compounds (gallic acid, protocatechuic acid, vanillic acid and syringic acid) is investigated using a synthesized mesoporous carbon on both single and multi-component synthetic solutions. Some correlation of the adsorption capacity of the carbon and the nature of adsorbate could be made, except for gallic acid whose concentration decrease seems to be not exclusively due to adsorption but also to polymerization reaction. In the multi-component mixture, negative effects in the adsorption capacity are observed probably due to competition for the active centers of the adsorbent surface. In desorption studies, ethanol presents better performance than water and acetonitrile. Vanillic acid is the compound with the higher adsorption and interestingly it is then possible to desorb a relatively high amount of it from the adsorbent, which may represent a possibility for a selective recovery of vanillic acid. These results present a potential way to treat the wastewater from the cork industry.

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Cordeiro, T, Castiñeira C, Mendes D, Florence Danède, Sotomayor J, Fonseca IM, Gomes da Silva M, Paiva A, Barreiros S, Cardoso MM, Viciosa MT, Correia NT, Dionisio M.  2017.  Stabilizing Unstable Amorphous Menthol through Inclusion in Mesoporous Silica Hosts. Molecular Pharmaceutics. 14:3164-3177., Number 9 AbstractWebsite
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Bernardo, MMS, Madeira CAC, dos Santos Nunes NCL, Dias DACM, Godinho DMB, de Jesus Pinto MF, do Nascimento Matos IAM, Carvalho APB, de Figueiredo Ligeiro Fonseca IM.  2017.  Study of the removal mechanism of aquatic emergent pollutants by new bio-based chars, Oct. Environmental Science and Pollution Research. 24:22698–22708., Number 28 AbstractWebsite

This work is dedicated to study the potential application of char byproducts obtained in the gasification of rice husk (RG char) and rice husk blended with corn cob (RCG char) as removal agents of two emergent aquatic contaminants: tetracycline and caffeine. The chars presented high ash contents (59.5–81.5{%}), being their mineral content mainly composed of silicon (as silica) and potassium. The samples presented a strong basic character, which was related to its higher mineral oxides content. RCG char presented better textural properties with a higher apparent surface area (144 m2 g−1) and higher micropore content (V micro = 0.05 cm3 g−1). The alkaline character of both chars promoted high ecotoxicity levels on their aqueous eluates; however, the ecotoxic behaviour was eliminated after pH correction. Adsorption experiments showed that RG char presented higher uptake capacity for both tetracycline (12.9 mg g−1) and caffeine (8.0 mg g−1), indicating that textural properties did not play a major role in the adsorption process. For tetracycline, the underlying adsorption mechanism was complexation or ion exchange reactions with the mineral elements of chars. The higher affinity of RG char to caffeine was associated with the higher alkaline character presented by this char.

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Sharipova, AA, Aidarova SB, Bekturganova NY, Tleuova A, Kerimkulova M, Yessimova O, Kairaliyeva T, Lygina O, Lyubchik S, Miller R.  2017.  Triclosan adsorption from model system by mineral sorbent diatomite. Colloids and Surfaces A: Physicochemical and Engineering Aspects. 532:97-101. AbstractWebsite

Adsorption of model systems of triclosan by mineral sorbent diatomite is studied. The triclosan equilibrium concentration was measured spectrophotometrically, the morphology of the diatomite characterized using scanning electron microscopy and the amount of the adsorbed triclosan on the diatomite quantified by a mass balance. Adsorption isotherms were analyzed according to the linear/nonlinear form of Langmuir, Freundlich, Sips and Toth isotherm models isotherms, using AMPL software. It is shown that nonlinear Langmuir and Sips isotherm model provided suitable fitting results and no pronounced difference in adsorption efficiency between isotherms measured after 1, 2 and 3days adsorption was observed. Determined maximum adsorption capacity of diatomite towards triclosan qs is 140mg/g. Averaged calculated values of ΔG are −9.9 and −9.6kJ/mol for Langmuir and Sips models respectively. The negative sign of such values indicates spontaneous, physical in nature adsorption.

Sharipova, AA, Aidarova SB, Bekturganova NE, Tleuova A, Schenderlein M, Lygina O, Lyubchik S, Miller R.  2016.  Triclosan as model system for the adsorption on recycled adsorbent materials. Colloids and Surfaces A: Physicochemical and Engineering Aspects. 505:193-196. AbstractWebsite

The adsorption of triclosan as model system was studied to qualify activated carbon sorbents recycled from gas masks (civilian gas mask GP5). The triclosan equilibrium concentration was measured spectrophotometrically, the morphology of the activated carbon characterized by scanning electron microscopy, and the amount of the adsorbed triclosan on the activated carbon quantified by a mass balance method. Experimental isotherms were fitted by Langmuir, Freundlich and Sips adsorption models. It was obtained that the contact time is a crucial sorption parameter that provides information on the optimum adsorption efficiency. It was shown that the maximum efficiency of GP5 (88%) is obtained after 10days of adsorption at a maximal concentration of triclosan and carbon loading 1mg/l. No significant adsorption efficiency differences were measured after 5 and 10days of adsorption. The non-linear Sips isotherm, a combined Freundlich–Langmuir model, provides suitable fitting results. The observed remarkable adsorption capacity of activated carbon (GP5) towards triclosan adsorption (∼85mg/g) makes it a viable solution for wastewater treatment.

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Lourenço, SC, Torres CAV, Nunes D, Duarte P, Freitas F, Reis MAM, Fortunato E, Moldão-Martins M, da Costa LB, Alves VD.  2017.  Using a bacterial fucose-rich polysaccharide as encapsulation material of bioactive compounds. International Journal of Biological Macromolecules. 104:1099-1106. AbstractWebsite

The potential of a bacterial exopolysaccharide named FucoPol, produced by the bacterium Enterobacter A47, as encapsulation matrix was explored. Spherical capsules with a smooth surface were produced by spray drying. The obtained microcapsules had average diameters ranging from 0.5 to 26.7μm and presented thin walls (thickness from 222 to 1094nm). The capsules were loaded with two bioactive compounds: gallic acid (GA) and oregano essential oil (OEO). Both bioactive materials were encapsulated in FucoPol particles, retaining their antioxidant activity after the drying process. Release studies showed that GA release in simulated gastric and intestinal fluids was faster than that of OEO, envisaging that the latter had established stronger interactions with the polymer matrix. These results suggest that FucoPol has a good potential for use as encapsulating material of bioactive compounds for application in several areas, including food, cosmetic or pharmaceutical products.