Effect of extraction methods on kinetic,chemical composition and antibacterial activities of Tunisian Thymus vulgaris. L. essential oil

The present study aims to compare two innovative extraction techniques: microwave-assisted hydrodistillation (MAHD) and solvent-free microwave extraction (SFME) through traditional extraction techniques: hydrodistillation (HD) and steam distillation (SD) for their efficiency in the extraction of the volatile compounds from Tunisian Thymus vulgaris leaves; the kinetic, yield, composition and antibacterial activities of the essential oil were assessed in vitro. Results show that the essential oils extracted by microwaves were quantitatively (yield) similar to those obtained through the conventional methods, but qualitatively, essential oils analysed by gas chromatography–mass spectrometry (GC–MS) presented 17, 11, 11 and 8 compounds obtained through SFME, MAHD, SD and HD, respectively, mostly consisting of carvacrol (89.24–41.17%), followed by γ-terpinene (11.37–1.37%) and para-cymene (27.95–2.05%). The essential oils were screened for antibacterial activity against 5 microorganisms. All essential oils obtained by studied extraction methods showed the same resistance against Gram (?) and Gram (+) bacteria. The SFME method gave the best results: rapid kinetic of extraction (30 min vs. 35 min for MAHD, 120 min for SD, and 180 min for HD), less energy saving and cleanest process.     

High efficiency of methylene blue removal using a novel low-cost acid treated forest wastes,Cupressus semperirens cones: Experimental results and modeling

The removal of methylene blue (MB) from aqueous solutions using sulfuric acid modified Cupressus semperirens cones (H₂SO₄-CSC), was investigated. Results showed that a pH value of 12 was favorable for the adsorption of MB and that the moisture and ash yields are suitable for industrial exploitation. A high porosity value was found, 68.1%. In agreement with its low content of basicity compared to its acidity, the H₂SO4-CSC absorbent had an acidic behavior. Rate constants of pseudo-first-order, pseudo-second-order, and nth kinetic model were determined to analyze the dynamic of the biosorption process; they showed that adsorption kinetics followed a pseudo-second-order and nth kinetic models. Ionic strength was shown to have a negative impact on the biosorption of MB onto H₂SO₄-CSC. The Sips isotherm model was found to be the most relevant to describe MB biosorption onto H₂SO₄-CSC with a correlation factor R²?>?0.999. The biosorption capacity of H₂SO₄-CSC was found to be 460?mg?g^?1 at 10°C and 590?mg?g^?1 at 25°C, confirming biosorbent efficiency for the removal of MB dye from aqueous solutions. Thermodynamic parameters indicated that the biosorption process of MB was endothermic and more effective at high temperatures. The values of ΔG° and ΔH° confirmed that the biosorption of MB onto H₂SO₄-CSC was spontaneous and endothermic in nature. An irregular increase in randomness at the H₂SO₄-CSC–solution interface during the biosorption process was suggested by the positive values of ΔS°.     

Removal of Copper(II) from a Concentrated Sulphate Medium by Cloud Point Extraction Using an N,N′-Bis(salicylaldehyde)Ethylenediimine Di-Schiff Base Chelating Ligand

Various chelating ligands have been investigated for the cloud point extraction of several metal ions. However, limited studies on the use of the Schiff base ligands have been reported. In this work, cloud point extraction behavior of copper(II) with N,N′‐bis(salicylaldehyde)Ethylenediimine Schiff base chelating ligand, (H₂SALEN), was investigated in aqueous concentrated sulphate medium. The extraction process used is based on the formation of hydrophobic H₂SALEN–copper(II) complexes that are solubilized in the micellar phase of a non‐ionic surfactant, i.e. ethoxylated (9.5EO) tert‐butylphenol. The copper(II) complexes are then extracted into the surfactant‐rich phase above cloud point temperature. Different parameters affecting the extraction process of Cu(II), such as equilibrium pH, extractant concentration, and non‐ionic surfactant concentration were explored. The extraction of Cu(II) was studied in the pH range of 2–11. The results obtained showed that it was profoundly influenced by the pH of the aqueous medium. The concentration factor, C_f, of about 17 with extraction efficiency of E % ≈100 was achieved. The stoichiometry of the extracted complex of copper(II) was ascertained by the Yoe–Jones method to give a composition of 1:1 (Cu:H₂L). The optimum conditions of the extraction‐removal have been established as the following: (1) 1.86 × 10^?3 mol/L ligand; (2) 3 wt% surfactant; (3) pH of 8 (4) 0.5 mol/L Na₂SO₄ and (5) temperature of 60 °C.     

Synthesis and Characterization of a Novel Series of Amphiphilic Mercapto-1,2,4-Triazole Schiff Base Ligands: Investigation of their Behavior in Hydro-Organic Solutions

A novel series of four Schiff base amphiphiles derived from 3-mercapto-1,2,4-triazole and different alkyl chains were successfully prepared by a new synthetic three-step method. The chemical structures of the different ligands were characterized by elemental analysis, FT-IR spectroscopy, ¹H-NMR and ¹³C-NMR spectra. The effect of the chain length on the solution behavior of the amphiphilic ligands were studied, in both homogeneous and heterogeneous systems, using pH-metric and spectrophotometric methods. Based on the electronic spectroscopy data, some parameters governing their surfactant properties, such as the critical micelle concentration (CMC), the micellization free energy (ΔG _mic) and the hydrophilic-lipophilic balance (HLB) were evaluated in chloroform and discussed. The behavior of the four Schiff bases in the heterogeneous chloroform-water mixture was then explored through the establishment of their acidity (pK_A) and distribution (Log K _d) constants in 1 M chloride medium and the acidity constants in aqueous medium (pK_a) were deduced. Results showed that an increase of the alkyl chain decreases the distribution of the ligands and increases their acidity. The extractive performance of the Schiff base amphiphiles were investigated towards Ni(II) from a chloride medium at 30 °C. The analysis of extraction data revealed that the synthesized Schiff bases exhibit a better and faster extractability than many ligands reported in the literature.     

Impact of Microwave Assisted Infusion on the Quality and Volatile Composition of Olive Oil Aromatized with Rosemary Leaves

Olive oil with rosemary leaves by microwave assisted infusion (MAI) as an alternative to conventional infusion (CI) was evaluated. Microwave heating was applied to the mixture in order to accelerate diffusion of the rosemary volatile compounds into the olive oil. The volatile components of the aromatized oils were quantified by HS‐SPME/GC–MS, as well as several quality indexes such as free fatty acids (FFA), peroxide value (PV), specific coefficients of extinction, chlorophyll and carotenoid content, and color assessment. Fatty acid profiles of the oils aromatized by MAI were compared to those produced by CI. Results showed that the infusion time is reduced from 12 h to 10 min when utilizing MAI in place of CI. MAI treatment caused a slight increase in FFA levels, and specific extinction coefficient indices (K₂₃₂ and K₂₇₀). PV during MAI remained unchanged for the first 3 min, after which there was an observable increase. All physico‐chemical values were found to be well below the maximum permitted limits. The MAI treatment reduced chlorophyll and carotenoid levels during the final step of aromatization, thus affecting final color. The MAI aromatized oil was characterized by its clear green color (L*, a*, b* parameters). Fatty acid analysis showed that MAI slightly changed the fatty acid composition of the olive oil. This study indicates that MAI appears to be a viable and rapid method to flavor olive oil with rosemary leaves.     

Calcium alginate‐resistant starch mixed gel improved the survival of Bifidobacterium animalis subsp. lactis Bb12 and Lactobacillus rhamnosus LBRE‐LSAS in yogurt and simulated gastrointestinal conditions

The aim of this study was to investigate the protective effect of microencapsulation in calcium alginate‐resistant starch mixed gel of a new human isolated strain of Lactobacillus rhamnosus LBRE‐LSAS compared with the probiotic strain of Bifidobacterium animalis subsp. lactis Bb12. Influence of microencapsulation was tested under deleterious digestive environment, when challenged to salivary α‐amylase, to simulated gastric fluid and to simulated intestinal fluid. Bacterial survival, post‐acidifying activity and exopolysaccharides (EPS) content in stored mix yogurt were assessed. Integrity of the beads was acceptable under α‐amylase levels largely higher than those found in human saliva. Under simulated gastrointestinal model, viable cell counts of encapsulated cells were significantly higher than those observed with free cells and remained at the recommended levels. Additionally, microencapsulation allowed an improved viability of bacteria and generated higher EPS amounts in mix yogurt stored at 4 °C. Our results indicate that calcium alginate‐resistant starch beads extend survival under digestive conditions and in yogurt and could be used as an efficient delivery system for probiotics.     

Removal of tiemonium methylsulfate,from aqueous solutions using activated carbon prepared from date stones

The retention of a pharmaceutical compound, tiemonium methylsulfate (TIM), from aqueous solutions by adsorption onto activated carbon prepared from date stones (AC–DS) was investigated. Physical and chemical characteristics of this material were also determined. Results showed that pH 8 was optimal for TIM adsorption. Among the kinetic models considered, the pseudo-second-order model was the most appropriate to describe experimental data. Regarding adsorption isotherms, it was shown that the Sips model accurately describe the sorption of TIM onto AC–DS with a correlation factor R²?>?0.98. The adsorption capacity of AC–DS was found to be 42.2?mg?g^?1 at 10°C and 60.5?mg?g^?1 at 25°C, confirming its efficiency for the removal of this compound from aqueous solutions. The values of ΔG⁰ and ΔH⁰ confirmed that the adsorption of TIM onto AC–DS was spontaneous and endothermic in nature and hence more effective at high temperatures. An irregular increase in the randomness was suggested at the AC–DS solution interface during the adsorption process for positive values of ΔS⁰.