Inclusion of Natural Antioxidants of Mango Leaves in Porous Ceramic Matrices by Supercritical CO2 Impregnation.

Mango is one of the most important, medicinal tropical plants in the world from an economic point of view due to the presence of effective bioactive substances as co-products in its leaves. The aim of this work was to enhance the impregnation of natural antioxidants from mango leaves into a porous ceramic matrix. The effects of pressure, temperature, impregnation time, concentration of the extract and different porous silica on impregnation of phenolic compounds and antioxidant activity were analyzed. The volume of the pressurized fluid extract and amount of porous ceramic matrix remained constant. The best impregnation conditions were obtained at 6 h, 300 bar, 60 mg/mL, 35 °C and with MSU-H porous silica. The results indicated that increasing the pressure, concentration of the extract and temperature during impregnation with phenolic compounds such as gallic acid and iriflophenone 3-C (2-O-p-hydroxybenzolyl)-ß-D-glucoside increased the antioxidant activity and the amount of total phenols.

Application of Citrus By-Products in the Production of Active Food Packaging.

Some citrus by-products such as orange peel contains valuable compounds that could be recovered and restored into the food chain. In this study, an efficient valorization of orange peel has been investigated using green extraction, fractionation, and impregnation techniques. The first step included its extraction using CO2 and ethanol under different pressure (200-400 bar) and temperature (35-55 °C) conditions. The extracts obtained at 300 bar and 45 °C showed strong antioxidant with moderate antimicrobial activity. Then, the extract was subjected to a sequential fractionation process. The fraction obtained at 300 bar, 45 °C, and using 32% ethanol showed the strongest antioxidant and antimicrobial activity with a high extraction yield. Finally, the potential of the two best extracts (obtained at 400 bar and 45 °C before any fractionation and the fractions obtained at 300 bar, 45 °C using 32% ethanol) was determined by conducting an impregnation process to obtain an antioxidant food-grade rigid plastic that would preserve fresh food. The percentage of cosolvent (1 and 2% ethanol), the impregnation time (1 and 3 h), the pressure (200 and 400 bar), and the temperature (35 and 55 °C) were evaluated as variables of this process. The impregnated plastic showed good antioxidant and antimicrobial activities.

Effect of the Heating Rate to Prevent the Generation of Iron Oxides during the Hydrothermal Synthesis of LiFePO4.

Lithium-ion batteries (LIBs) have gained much interest in recent years because of the increasing energy demand and the relentless progression of climate change. About 30% of the manufacturing cost for LIBs is spent on cathode materials, and its level of development is lower than the negative electrode, separator diaphragm and electrolyte, therefore becoming the "controlling step". Numerous cathodic materials have been employed, LiFePO4 being the most relevant one mainly because of its excellent performance, as well as its rated capacity (170 mA·h·g-1) and practical operating voltage (3.5 V vs. Li+/Li). Nevertheless, producing micro and nanoparticles with high purity levels, avoiding the formation of iron oxides, and reducing the operating cost are still some of the aspects still to be improved. In this work, we have applied two heating rates (slow and fast) to the same hydrothermal synthesis process with the main objective of obtaining, without any reducing agents, the purest possible LiFePO4 in the shortest time and with the lowest proportion of magnetite impurities. The reagents initially used were: FeSO4, H3PO4, and LiOH, and a crucial phenomenon has been observed in the temperature range between 130 and 150 °C, being verified with various techniques such as XRD and SEM.

Potential Use of Annona Genus Plants Leaf Extracts to Produce Bioactive Transdermal Patches by Supercritical Solvent Impregnation.

The objective of the present work was to develop a bioactive transdermal patch functionalized with Annona leaf extracts (ALE) by means of supercritical impregnation technique. The potential of six different Annona leaf extracts (ALE) obtained with the enhanced solvent system formed by carbon dioxide + ethanol/acetone was evaluated taking into account the antioxidant activity, total phenol composition and global extraction yields. For the impregnation of ALE, two drug supporting systems were tested: hydrocolloid sodium carboxymethyl cellulose (NaCMC) and polyester dressings (PD). The effect of the impregnation conditions, including pressure (P), temperature (T), percent of co-solvent (ethanol) and ALE/polymer mass ratio, was determined with regard to the loading and the functional activity of the impregnated samples. The optimal impregnation conditions of ALE were established at 55 °C and 300 bar which led to obtained transdermal patches with antioxidant and antimicrobial capacity. In order to understand the behavior of the process, the homogeneity of the samples in the vessels was also evaluated. The best results were obtained at higher proportions of co-solvent in the system.

Application of a Natural Antioxidant from Grape Pomace Extract in the Development of Bioactive Jute Fibers for Food Packaging.

There is an increasing demand for the use of new food packaging materials. In this study, natural jute fibers impregnated with a Petit Verdot Red Grape Pomace Extract (RGPE) was proposed as a new active food packaging material. Pressurized Liquid Extraction (PLE) and Enhanced Solvent Extraction (ESE) techniques were employed to obtain the bioactive RGPE. Afterward the supercritical solvent impregnation conditions to obtain RGPE-natural jute fibers were studied, by varying pressure, modifier percentage and dried RGPE mass. PLE technique offered the highest bioactive extract at 20 MPa, 55 °C, 1 h residence time using C2H5OH:H2O (1:1 v/v), providing an EC50 of 3.35 ± 0.25 and antibacterial capacity against Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa (MIC of 12.0, 1.5 and 4.0 mg/mL RGPE respectively). The natural jute fibers impregnated with 3 mL of that RGPE (90 mg/mL) at 50 MPa and 55 °C generated the most efficient packing material with regards to its food preservation potential.

Foaming of Polycaprolactone and Its Impregnation with Quercetin Using Supercritical CO2.

Foamed polycaprolactone impregnated with quercetin was carried out with a batch foaming technique using supercritical CO2. The experimental design was developed to study the influence of pressure (15-30 MPa), temperature (308-333 K), and depressurization rate (0.1-20) on the foam structure, melting temperature, and release tests of composites. The characterization of the experiments was carried out using scanning electron microscopy, X-ray diffractometer, and differential scanning calorimetry techniques. It was observed that the porosity created in the polymer had a heterogeneous structure, as well as the impregnation of the quercetin during the process. On the other hand, controlled release tests showed a significant delay in the release of quercetin compared to commercial quercetin.

Helikaurolides A-D with a Diterpene-Sesquiterpene Skeleton from Supercritical Fluid Extracts of Helianthus annuus L. var. Arianna.

Four novel compounds (1-4) with an unprecedented skeleton that combines a sesquiterpene lactone and a kaurane diterpene acid were isolated from Helianthus annuus L. var. Arianna extract, which was obtained under supercritical conditions. The structures of 1-4 were elucidated by NMR and MS analyses. The biosynthetic routes involve sesquiterpene lactones and kauranic acid, both of which were previously isolated from this species.

Isolation of Bioactive Compounds from Sunflower Leaves (Helianthus annuus L.) Extracted with Supercritical Carbon Dioxide.

The work described herein is a continuation of our initial studies on the supercritical fluid extraction (SFE) with CO2 of bioactive substances from Helianthus annuus L. var. Arianna. The selected SFE extract showed high activity in the wheat coleoptile bioassay, in Petri dish phytotoxicity bioassays, and in the hydroponic culture of tomato seeds. Chromatographic fractionations of the extracts and a spectroscopic analysis of the isolated compounds showed 52 substances belonging to 10 different chemical classes, which were mainly sesquiterpene lactones, diterpenes, and flavonoids. Heliannuol M (31), helivypolides K and L (36, 37), and helieudesmanolide B (38) are described for the first time in the literature. Metabolites have been tested in the etiolated wheat coleoptile bioassay with good results in a noteworthy effect on germination. The most active compounds were also tested on tomato seeds, heliannuol A (30) and leptocarpin (45) being the most active, with values similar to those of the commercial herbicide.

Green extraction of antioxidants from different varieties of red grape pomace.

The extraction yield, phenolic content, anthocyanin content and antioxidant activity of extracts from different varieties of red grapes, Cabernet Sauvignon, Merlot, Petit Verdot, Syrah, Tempranillo and Tintilla, using pressurized green solvents have been analyzed. Two techniques were studied and compared: supercritical fluid extraction (SFE) with CO2 + 20% ethanol and pressurized liquid extraction (PLE) with either ethanol, water or an ethanol/water mixture as the extraction solvents. The Petit Verdot variety allowed the highest global and phenolic yield, and antioxidant activity. The best conditios for PLE obtained from the experimental design and kinetic study were 50% ethanol/water as the pressurized solvent at 90 bar, 120 °C, a flow rate of 5 g/min and, an extraction time of 90 min. A statistical analysis of variance has been performed and it was found that temperature is the only variable that has a statistical influence on the extraction yield. The antioxidant activity levels of the extracts are very promising and they are similar to those obtained with the antioxidant tocopherol.

High pressure extraction of antioxidants from Solanum stenotomun peel.

In the work described here, two techniques for the recovery of anthocyanins from potato peel were studied and compared. One of the techniques employed was supercritical fluid extraction (SFE) with pure CO2 or with CO2 and ethanol as cosolvent and the other technique was pressurized liquid extraction (PLE), where the solvent used was ethanol in water acidified to pH 2.6. The effects of pressure and temperature were studied and the anthocyanin contents obtained were statistically analyzed. In SFE the use of low pressure (100 bar) and high temperature (65 °C) was desirable for the anthocyanin extraction. With PLE the anthocyanin contents are increased considerably, and the best yields were obtained at 100 bar and 80 °C. This result is in correspondence with antioxidant activity index values (1.66) obtained in a DPPH antioxidant activity assay. In the extracts obtained with PLE the phenolic compounds were also determined, but the main compounds presented in the extract are anthocyanins.

SFE kinetics of bioactive compounds from Helianthus annuus L.

The kinetics of the supercritical fluid extraction of bioactive compounds from sunflower using CO(2) as solvent were studied in order to establish an efficient method for this extraction. The influence of time of extraction at different solvent flow rates was investigated. The extraction pressure and temperature were optimized in previous studies and these values used were 400 bar and 50 degrees C. The extraction yields and the bioactivity levels of the extracts were also analysed. The results indicate that the most appropriate extraction time is between 120 and 180 min depending on the solvent flow and the pretreatment of the sample. The dried sample extracted at 40 g/min, the congealed sample extracted at the same flow and 180 min, and the dried sample extracted at 25 g/min for 120 min showed the best activity profiles. The extractions were carried out in a pilot plant with an extraction vessel with a capacity of 2 L.

Supercritical CO(2) extraction of PAHs on spiked soil Co-solvent effect and solvent regeneration by ozonization.

The supercritical CO(2) extraction of four PAHs (acenaphthene, phenanthrene, anthracene and fluoranthene) from an artificially contaminated soil has been investigated. The effect of temperature (40-60 degrees C), pressure (300-500 bar) and extraction time (90-150 min) has been assessed by conducting a Box-Behnken experimental design. The results suggest the existence of perturbation variables other than the aforementioned controlled variables leading to a significant dispersion of extraction recoveries. With the exception of anthracene, an optimum in temperature (50 degrees C) is envisaged when extracting the PAHs. Analogously, with the exception of anthracene (positive effect), pressure does not have a significant influence. The recovery yield increases as extraction time is increased to a value of 120 min. No further improvement is experienced thereafter. If a co-solvent is used (H(2)O(2) aqueous solution) a beneficial effect can be noticed. Hydrogen peroxide concentration did exert no significant influence in the process. Methanol used to collect the extracted PAHs could be regenerated by gaseous ozone and reused in several consecutive runs.