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 degrees C) conditions. The extracts obtained at 300 bar and 45 degrees 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 degrees 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 degrees C before any fractionation and the fractions obtained at 300 bar, 45 degrees 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 degrees C) were evaluated as variables of this process. The impregnated plastic showed good antioxidant and antimicrobial activitiesWe gratefully acknowledge the Spanish Ministry of Science and Technology (Project CTQ2014-52427-R) for its financial support through FEDER (European Funds for Regional Development)

Supercritical Impregnation of Ketoprofen into Polylactic Acid for Biomedical Application: Analysis and Modeling of the Release Kinetic

Ketoprofen (KET) is an anti-inflammatory drug often used in medicine due to its analgesic and antipyretic effects. If it is administered in a controlled form by means of different dosing devices, it acts throughout the patient's recovery period improving its efficacy. This study intends to support the use of supercritical solvent impregnation (SSI) as an efficient technique to develop polylactic acid (PLA) functionalized with ketoprofen, for use as controlled drug release devices. For this purpose, firstly, the influence of different SSI variables on the desirable swelling of the polymer structure, while avoiding their foaming, were evaluated. Then, the resulting ketoprofen loading was evaluated under different pressure/temperature conditions. It was generally found that as pressure and temperature are higher, the drug impregnation loads also increase. The maximum impregnation loads (at about 9% KET/PLA) were obtained at 200 bar and 75 degrees C. In vitro drug release tests of the impregnated compound were also carried out, and it was found that drug release profiles were also dependent on the specific pressure and temperature conditions used for the impregnation of each polymer filament

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 di ractometer, and di erential 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

Supercritical Impregnation of PLA Filaments with Mango Leaf Extract to Manufacture Functionalized Biomedical Devices by 3D Printing

Polylactic Acid (PLA) filaments impregnated with ethanolic mango leaves extract (MLE) with pharmacological properties were obtained by supercritical impregnation. The effects of pressure, temperature and amount of extract on the response variables, i.e., swelling, extract loading and bioactivity of the PLA filaments, were determined. The analysis of the filaments biocapacities revealed that impregnated PLA filaments showed 11.07% antidenaturant capacity and 88.13% antioxidant activity, which after a 9-day incubation shifted to 30.10% and 9.90%, respectively. Subsequently, the same tests were conducted on printed samples. Before their incubation, the printed samples showed 79.09% antioxidant activity and no antidenaturant capacity was detected. However, after their incubation, the antioxidant activity went down to only 2.50%, while the antidenaturant capacity raised up to 23.50%. The persistence of the bioactive properties after printing opens the possibility of using the functionalized PLA filaments as the feed for a three-dimensional (3D) printer.This work is part of a project granted by the Junta de Andalucia (P18-RT-3272) through its financing by the FEDER funds 2014-2020

Deposition of CAP/Antioxidants Systems on Silica Particles Using the Supercritical Antisolvent Process

Supercritical carbon dioxide has been used to deposit co-precipitates of natural antioxidants with a polymer onto silica microparticles. The supercritical antisolvent process (SAS) was carried out with the antioxidants by introducing the silica microparticles into the precipitator vessel. Two di erent configurations were employed to pump the solution. In one configuration, the antioxidant and the polymer were dissolved and injected together through a nozzle. In the second configuration, the antioxidant and the polymer were dissolved in di erent solutions and sprayed through di erent nozzles. The use of operating conditions significantly above the critical point (180 bar and 323 K) led to the formation of composites made up of co-precipitates and silica. Delivery profiles showed that the presence of the polymer and the silica delayed release of the antioxidant into gastric media, thus protecting it and allowing its full delivery to the intestinal fluids to improve the e ectiveness of the antioxidant

Analysis of the Supercritical Water Gasification of Cellulose in a Continuous System Using Short Residence Times

Supercritical Water Gasification (SCWG) has the capacity to generate fuel gas effluent from wet biomass without previously having to dry the biomass. However, substantial efforts are still required to make it a feasible and competitive technology for hydrogen production. Biomass contains cellulose, hemicellulose and lignin, so it is essential to understand their behavior in high-pressure systems in order to optimize hydrogen production. As the main component of biomass, cellulose has been extensively studied, and its decomposition has been carried out at both subcritical and supercritical conditions. Most previous works of this model compound were carried out in batch reactors, where reaction times normally take place in a few minutes. However, the present study demonstrates that gasification reactions can achieve efficiency levels of up to 100% in less than ten seconds. The effect of temperature (450-560 degrees C), the amount of oxidant (from no addition of oxidant to an excess over stoichiometric of 10%, n = 1.1), the initial concentration of organic matter (0.25-2 wt.%) and the addition of a catalyst on the SCWG of cellulose in a continuous tubular reactor at short residence times (from 6 to 10 s) have been studied in this work. Hydrogen yields close to 100% in the gas phase were obtained when operating under optimal conditions. Moreover, a validation of the experimental data has been conducted based on the theoretical data obtained from its kinetics

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 degrees 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.The authors would like to thank the research group in "The Institute for Mediterranean and Subtropical Horticulture La Mayora (IHSM)" (CSIC, Malaga, Spain) for providing the raw material and for their support. This research was funded by Junta de Andalucia-FEDER funds 2014-2020, project P18-RT-3272, the Spanish Ministry of Science and Technology, project CTQ2017-86661-R and the European Regional Development Fund(ERDF)

Determining the Optimal Conditions for the Production by Supercritical CO2 of Biodegradable PLGA Foams for the Controlled Release of Rutin as a Medical Treatment

Poly(D,L,-lactide-co-glycolide) (PLGA) foam samples impregnated with rutin were successfully produced by supercritical foaming processes. A number of parameters such as pressure (80–200 bar), temperature (35–55 C), depressurization rate (5–100 bar/min), ratio lactide:glycolide of the poly(D,L,-lactide-co-glycolide) (50:50 and 75:25) were studied to determine their effect on the expansion factor and on the glass transition temperature of the polymer foams and their consequences on the release profile of the rutin entrapped in them. The impregnated foams were characterized by scanning electron microscopy, differential scanning calorimetry, and mercury intrusion porosimetry. A greater impregnation of rutin into the polymer foam pores was observed as pressure was increased. The release of rutin in a phosphate buffer solution was investigated. The controlled release tests confirmed that the modification of certain variables would result in considerable differences in the drug release profiles. Thus, five-day drug release periods were achieved under high pressure and temperature while the depressurization rate remained low.This research was funded by Spanish Ministry of Economy, Industry and Competitiveness: CTQ2017-86661-R

From olive leaves to spherical nanoparticles by one-step RESS process precipitation

In this work, spherical nanoparticles to be used in cosmetic, agro food or pharmaceutical industries have been directly precipitated from olives leaves in one-step RESS process. The leaves were brought into contact with supercritical CO2, and a fraction of the compounds from the flavone and flavonol families that can be found in the leaves were dissolved; then, by depressurizing the vessel, these compounds formed particles in the nanometer range. A complete factorial design was generated to thoroughly determine the influence from the main parameters on the RESS process with respect to the precipitated nanoparticles and their heterogeneity. Their antioxidant activity was also evaluated. Different pressures (250-350 bar), temperatures (60 and 100 degrees C), leaves sample weights (2 and 4 g) and cosolvent volumes, namely ethanol (9 and 18 mL), were studied as the main parameters that could affect the solvation and precipitation of the particle with active compounds in the leaves. Other parameters such as contact time (1 h) or nozzle size diameter (100 mu m) remained unchanged. The antioxidant activity was evaluated by means of the radical scavenging method using the radical 2,2-diphenyl-1-picrylhydrazole (DPPH). Spherical particles with diameters in the range of 55 nm to 4 mu m were obtained. Lower pressures and higher temperatures seemed to result in a reduction of the mean particle size. Greater volume of cosolvent is also recommended to reduce mean particle size. However, lower pressure, temperature and volume of cosolvent seems to promote a greater homogeneity of the particles. By means of chromatographic analyses, the main compounds, responsible for the antioxidant activity, such as oleuropein, quercetin or apigenin among others were identified

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