3 resultados para separation and preconcentration

em Instituto Politécnico de Bragança


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The production of natural extracts requires suitable processing conditions to maximize the preservation of the bioactive ingredients. Herein, a microwave-assisted extraction (MAE) process was optimized, by means of response surface methodology (RSM), to maximize the recovery of phenolic acids and flavonoids and obtain antioxidant ingredients from tomato. A 5-level full factorial Box-Behnken design was successfully implemented for MAE optimization, in which the processing time (t), temperature (T), ethanol concentration (Et) and solid/liquid ratio (S/L) were relevant independent variables. The proposed model was validated based on the high values of the adjusted coefficient of determination and on the non-significant differences between experimental and predicted values. The global optimum processing conditions (t=20 min; T=180 ºC; Et=0 %; and S/L=45 g/L) provided tomato extracts with high potential as nutraceuticals or as active ingredients in the design of functional foods. Additionally, the round tomato variety was highlighted as a source of added-value phenolic acids and flavonoids.

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In order to evaluate the impact of the alkyl side chain length and symmetry of the cation on the thermophysical properties of water-saturated ionic liquids (ILs), densities and viscosities as a function of temperature were measured at atmospheric pressure and in the (298.15 to 363.15) K temperature range, for systems containing two series of bis(trifluoromethylsulfonyl)imide-based compounds: the symmetric [C n C n im][NTf2] (with n = 1-8 and 10) and asymmetric [C n C1im][NTf2] (with n = 2-5, 7, 9 and 11) ILs. For water-saturated ILs, the density decreases with the increase of the alkyl side chain length while the viscosity increases with the size of the aliphatic tails. The saturation water solubility in each IL was further estimated with a reasonable agreement based on the densities of water-saturated ILs, further confirming that for the ILs investigated the volumetric mixing properties of ILs and water follow a near ideal behaviour. The water-saturated symmetric ILs generally present lower densities and viscosities than their asymmetric counterparts. From the experimental data, the isobaric thermal expansion coefficient and energy barrier were also estimated. A close correlation between the difference in the energy barrier values between the water-saturated and pure ILs and the water content in each IL was found, supporting that the decrease in the viscosity of ILs in presence of water is directly related with the decrease of the energy barrier.

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In this work, ionic liquids are evaluated for the first time as solvents for extraction and entrainers in separation processes involving terpenes and terpenoids. For that purpose, activity coefficients at infinite dilution, γ13 ∞, of terpenes and terpenoids, in the ionic liquids [C4mim]Cl, [C4mim][CH3SO3], [C4mim][(CH3)2PO4] and [C4mim][CF3SO3] were determined by gas−liquid chromatography at six temperatures in the range 398.15 to 448.15 K. On the basis of the experimental values, a correlation of γ13 ∞ with an increase of the solubility parameters is proposed. The infinite dilution thermodynamic functions were calculated showing the entropic effect is dominant over the enthalpic. Gas−liquid partition coefficients give indications about the recovery and purification of terpenes and terpenoids from ionic liquid solutions. Presenting a strong innovative character, COSMO-RS was evaluated for the description of the selectivities and capacities, showing to be a useful tool for the screening of ionic liquids in order to find suitable candidates for terpenes and terpenoids extraction, and separation. COSMO-RS predictions show that in order to achieve the maximum separation efficiency, polar anions should be used such as bis(2,4,4-trimethylpentyl)phosphinate or acetate, whereas high capacities require nonpolar cations such as phosphonium.