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The food industry has a current challenge of increasing the recycling of post-consumer plastics to reduce plastic waste towards a circular economy, especially flexible polypropylene, which is highly demanded in food packaging. However, recycling post-consumer plastics is limited because service life and reprocessing degrade their physical-mechanical properties and modify the migration of components from the recycled material to the food. This research evaluated the feasibility of valorization of post-consumer recycled flexible polypropylene (PCPP) by incorporating fumed nanosilica (NS). For this purpose, the effect of concentration and type (hydrophilic and hydrophobic) of NS on the morphological, mechanical, sealing, barrier and overall migration properties of PCPP films was studied. Incorporating NS improved Young's modulus and, more significantly, tensile strength at 0.5 wt% and 1 wt%, where a better particle dispersion was confirmed by EDS-SEM, but it diminished elongation at breakage of the films. Interestingly, NS tended to increase the seal strength of PCPP nanocomposite films more significantly at higher NS content, showing a seal failure of the adhesive peel type which is preferred for flexible packaging. NS at 1 wt% did not affect the water vapor and oxygen permeabilities of the films. Overall migration of PCPP and nanocomposites exceeded the limit value of 10 mg dm-2 allowed by European legislation at the studied concentrations of 1% and 4 wt%. Nonetheless, NS reduced the overall migration of PCPP from 17.3 to 15 mg dm-2 in all nanocomposites. In conclusion, PCPP with 1 wt% of hydrophobic NS presented an improved overall performance of the studied packaging properties.

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Collection and mechanical recycling of post-consumer flexible polypropylene packaging is limited, principally due to polypropylene being very light-weight. Moreover, service life and thermal-mechanical reprocessing degrade PP and change its thermal and rheological properties according to the structure and provenance of recycled PP. This work determined the effect of incorporating two fumed nanosilica (NS) types on processability improvement of post-consumer recycled flexible polypropylene (PCPP) through ATR-FTIR, TGA, DSC, MFI and rheological analysis. Presence of trace polyethylene in the collected PCPP increased the thermal stability of the PP and was significantly maximized by NS addition. The onset decomposition temperature raised around 15 °C when 4 and 2 wt% of a non-treated and organically modified NS were used, respectively. NS acted as a nucleating agent and increased the crystallinity of the polymer, but the crystallization and melting temperatures were not affected. The processability of the nanocomposites was improved, observed as an increase in viscosity, storage and loss moduli with respect to the control PCPP, which were deteriorated due to chain scission during recycling. The highest recovery in viscosity and reduction in MFI were found for the hydrophilic NS due to a greater impact of hydrogen bond interactions between the silanol groups of this NS and the oxidized groups of the PCPP.

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In the present study, we report on the successful synthesis of hollow iron oxide nanospheres. The hollow Fe3O4 nanospheres were synthesized following a four-step procedure: electrospraying spherical PVP particles, coating these particles with alumina (Al2O3) and hematite (Fe2O3) through atomic layer deposition and, finally, a thermal reduction process to degrade the polymer (PVP) and convert hematite (Fe2O3) into magnetite (Fe3O4). A structural analysis using X-ray diffraction (XRD) confirmed the effectiveness of the thermal reduction process. A morphological analysis confirmed that the four-step procedure allowed for the obtainment of hollow iron oxide nanospheres, even though the reduction process caused a contraction in the diameter of the particles of almost 300 nm, but did not affect the thickness of the walls of the hollow spheres that remained at approximately 15 nm. Magnetic properties of the hollow iron oxide nanospheres enable their use in applications where the agglomeration of magnetic nanostructures in liquid media is commonly not allowed, such as in drug encapsulation and delivery.

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This review was focused on describing the combination of electrospinning and cyclodextrin inclusion complexes as one of the newest alternatives for the development of food packaging materials with antimicrobial and/or antioxidant properties. The advantages of this technological combination, the routes to design the active materials, the characterization and application of such materials were reviewed. Electrospinning has allowed developing active packaging materials composed by fibrillary structures with a high ratio surface-to-volume. On the other hand, cyclodextrin inclusion complexes have maintained the properties of active compounds when they have been incorporated in packaging materials. Both methods have been recently combined and novel active food packaging materials have been obtained through three different routes. Polymeric solutions containing preformed (route 1) or in-situ formed (route 2) cyclodextrin inclusion complexes have been electrospun to obtain packaging materials. Furthermore, cyclodextrin inclusion complexes solutions have been directly electrospun (route 3) in order to produce those materials. The developed packaging materials have exhibited a high active compound loading with a long lasting release. Therefore, the protection of different foodstuff against microbial growth, oxidation and quality decay as well as the maintenance of their physical and sensory properties have been achieved when those materials were applied as active packaging.

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The performance characteristics of polylactic acid (PLA) as an active food packaging film can be highly influenced by the incorporation of active agents (AAs) into PLA, and the type of processing technique. In this review, the effect of processing techniques and the addition of natural AAs on the properties related to PLA performance as a packaging material are summarized and described through a systematic analysis, giving new insights about the relation between processing techniques, types of AA, physical-mechanical properties, barriers, optical properties, compostability, controlled release, and functionalities in order to contribute to the progress made in designing antioxidant and antimicrobial PLA packaging films. The addition of AAs into PLA films affected their optical properties and influenced polymer chain reordering, modifying their thermal properties, functionality, and compostability in terms of the chemical nature of AAs. The mechanical and barrier performance of PLA was affected by the AA's dispersion degree and crystallinity changes resulting from specific processing techniques. In addition, hydrophobicity and AA concentration also modified the barrier properties of PLA. The release kinetics of AAs from PLA were tuned, modifying diffusion coefficient of the AAs in terms of the different physical properties of the films that resulted from specific processing techniques. Several developments based on the incorporation of antimicrobial and antioxidant substances into PLA have displayed outstanding activities for food protection against microbial growth and oxidation.

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Currently, reducing packaging plastic waste and food losses are concerning topics in the food packaging industry. As an alternative for these challenges, antimicrobial and antioxidant materials have been developed by incorporating active agents (AAs) into biodegradable polymers to extend the food shelf life. In this context, developing biodegradable active materials based on polylactic acid (PLA) and natural compounds are a great alternative to maintain food safety and non-toxicity of the packaging. AAs, such as essential oils and polyphenols, have been added mainly as antimicrobial and antioxidant natural compounds in PLA packaging. In this review, current techniques used to develop active PLA packaging films were described in order to critically compare their feasibility, advantages, limitations, and relevant processing aspects. The analysis was focused on the processing conditions, such as operation variables and stages, and factors related to the AAs, such as their concentrations, weight losses during processing, and incorporation technique, among others. Recent developments of active PLA-based monolayers and bi- or multilayer films were also considered. In addition, patents on inventions and technologies on active PLA-based films for food packaging were reviewed. This review highlights that the selection of the processing technique and conditions to obtain active PLA depends on the type of the AA regarding its volatility, solubility, and thermosensitivity.

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The deterioration of the physical-mechanical properties and loss of the chemical safety of plastics after consumption are topics of concern for food packaging applications. Incorporating nanoclays is an alternative to improve the performance of recycled plastics. However, properties and overall migration from polymer/clay nanocomposites to food require to be evaluated case-by-case. This work aimed to investigate the effect of organic modifier types of clays on the structural, thermal and mechanical properties and the overall migration of nanocomposites based on 50/50 virgin and recycled post-consumer polypropylene blend (VPP/RPP) and organoclays for food packaging applications. The clay with the most hydrophobic organic modifier caused higher thermal stability of the nanocomposites and greater intercalation of polypropylene between clay mineral layers but increased the overall migration to a fatty food simulant. This migration value was higher from the 50/50 VPP/RPP film than from VPP. Nonetheless, clays reduced the migration and even more when the clay had greater hydrophilicity because of lower interactions between the nanocomposite and the fatty simulant. Conversely, nanocomposites and VPP/RPP control films exhibited low migration values in the acid and non-acid food simulants. Regarding tensile parameters, elongation at break values of PP film significantly increased with RPP addition, but the incorporation of organoclays reduced its ductility to values closer to the VPP.

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The design of multilayer systems is an innovative strategy to improve physical properties of biodegradable polymers and introduce functionality to the materials through the incorporation of an active compound into some of these layers. In this work, a trilayer film based on a sandwich of electrospun polycaprolactone (PCL) fibers (PCLé) containing quercetin (Q) and cellulose nanocrystals (CNC) between extruded polylactic acid (PLA) films was designed with the purpose of improving thermal and barrier properties and affording antioxidant activity to packaged foods. PCLé was successfully electrospun onto 70 µm-thick extruded PLA film followed by the assembling of a third 25 µm-thick commercial PLA film through hot pressing. Optical, morphological, thermal, and barrier properties were evaluated in order to study the effect of PCL layer and the addition of Q and CNC. Bilayer systems obtained after the electrospinning process of PCL onto PLA film were also evaluated. The release of quercetin from bi- and trilayer films to food simulants was also analyzed. Results evidenced that thermal treatment during thermo-compression melted PCL polymer and resulted in trilayer systems with barrier properties similar to single PLA film. Quercetin release from bi- and trilayer films followed a similar profile, but achieved highest value through the addition of CNC.

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The inhibitory and bactericidal capacity of Listex P100 bacteriophage has been studied against different concentrations of Listeria monocytogenes in stationary and exponential phases. Three different matrices were employed to developed films incorporating Listex P100: (1) sodium caseinate, (2) sodium alginate mixed with gelatin, and (3) polyvinyl alcohol (PVOH). All the films were successfully developed by casting at room temperature. These active biodegradable films were optical, structural, and thermally characterized, and their antimicrobial capacities against L. monocytogenes were studied. The incorporation of phages did not affect the morphology, colour, opacity, and thermal stability of polymers. The antimicrobial analysis revealed the bacteriophage presented a high antimicrobial capacity against L. monocytogenes in the stationary phase (4.40 and 6.19 log reduction values or bactericide effect depending on the initial inoculum of the pathogen). Developed films showed antimicrobial capacity close to 1 log after 24 h of incubation at 30 °C. The effectiveness of PVOH films was greater under refrigeration conditions, reaching 2 log reduction after eight days of incubation. The use of these films as a coating in a food or as part of a packaging could improve food safety against the growth of pathogenic microorganisms such as Listeria monocytogenes.

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Nanotechnology is considered a highly valued technology to reduce the current environmental problem that is derived from plastic accumulation. The need to recycle and reuse packaging materials is essential to create a sustainable society towards a circular economy. However, the reprocessing of polymers leads to the deterioration of their characteristic mechanical, optical, thermal, and barrier properties due to the degradation of their polymeric chains. When recycled polymers are reinforced with nanoadditives, aforementioned properties improve and their use in the circular economy is more viable. In this review, different types of nanoadditives and recent advances in the development of recycled polymer nanocomposites reinforced with nanoadditives will be presented. In addition, there is a description of two research topics of current interest, recyclability of nanocomposites and safety for food packaging applications. Recyclability of nanocomposites requires a study that includes the nature of the polymer matrix, the type of polymer and the concentration of nanofiller, the morphology, the presence of additives, and the conditions of the thermal-mechanical cycles. Finally, safety section is dedicated to clarify the migration process in nanoreinforced-recycled polymers in order to assess their safety for food contact applications.

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The interest in the development of novel biodegradable composites has increased over last years, and multilayer composites allow the design of materials with functionality and improved properties. In this work, bilayer structures based on a coated zein layer containing quercetin and cellulose nanocrystals (CNC) over an extruded poly(lactic acid) (PLA) layer were developed and characterized. Bilayer composites were successfully obtained and presented a total thickness of approx. 90 µm. The coated zein layer and quercetin gave a yellowish tone to the composites. The incorporation of the zein layer containing CNC decreased the volatile release rate during thermal degradation. Regarding to mechanical properties, bilayer composites presented lower brittleness and greater ductility evidenced by a lower Young's modulus and higher elongation values. Water permeability values of bilayer composites greatly increased with humidity and the zein coated layer containing quercetin increased this effect. Experimental data of quercetin release kinetics from bilayer structures indicated a higher release for an alcoholic food system, and the incorporation of cellulose nanocrystals did not influence the quercetin diffusion process.

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The açaí fruit (Euterpe oleracea Mart.) is well known for its high content of antioxidant compounds, especially anthocyanins, which provide beneficial health properties. The incorporation of this fruit is limited to food products whose processing does not involve the use of high temperatures due to the low thermal stability of these functional components. The objective of this work was the encapsulation of açaí fruit antioxidants into electrosprayed zein, a heat-resistant protein, to improve their bioavailability and thermal resistance. First, the hydroalcoholic açaí extract was selected due to its high polyphenolic content and antioxidant capacities, and, subsequently, it was successfully encapsulated in electrosprayed zein particles. Scanning electron microscopy studies revealed that the resulting particles presented cavities with an average size of 924 nm. Structural characterization by Fourier transform infrared spectroscopy revealed certain chemical interaction between the active compounds and zein. Encapsulation efficiency was approximately 70%. Results demonstrated the effectiveness of the encapsulated extract on protecting polyphenolic content after high-temperature treatments, such as sterilization (121 °C) and baking (180 °C). Bioaccesibility studies also indicated an increase of polyphenols presence after in vitro digestion stages of encapsulated açaí fruit extract in contrast with the unprotected extract.

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The search for new antimicrobial substances has increased in recent years. Antimicrobial nanostructures are one of the most promising alternatives. In this work, titanium dioxide nanotubes were obtained by an atomic layer deposition (ALD) process over electrospun polyvinyl alcohol nanofibers (PVN) at different temperatures with the purpose of obtaining antimicrobial nanostructures with a high specific area. Electrospinning and ALD parameters were studied in order to obtain PVN with smallest diameter and highest deposition rate, respectively. Chamber temperature was a key factor during ALD process and an appropriate titanium dioxide deposition performance was achieved at 200 °C. Subsequently, thermal and morphological analysis by SEM and TEM microscopies revealed hollow nanotubes were obtained after calcination process at 600 °C. This temperature allowed complete polymer removal and influenced the resulting anatase crystallographic structure of titanium dioxide that positively affected their antimicrobial activities. X-ray analysis confirmed the change of titanium dioxide crystallographic structure from amorphous phase of deposited PVN to anatase crystalline structure of nanotubes. These new nanostructures with very large surface areas resulted in interesting antimicrobial properties against Gram-positive and Gram-negative bacteria. Titanium dioxide nanotubes presented the highest activity against Escherichia coli with 5 log cycles reduction at 200 µg/mL concentration.

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The main objective of this work was to study the release of cinnamaldehyde (CIN) from electrospun poly lactic acid (e-PLA) mats obtained through two techniques: (i) direct incorporation of active compound during the electrospinning process (e-PLA-CIN); and (ii) supercritical carbon dioxide (scCO2) impregnation of CIN within electrospun PLA mats (e-PLA/CINimp). The development and characterization of both of these active electrospun mats were investigated with the main purpose of modifying the release kinetic of this active compound. Morphological, structural, and thermal properties of these materials were also studied, and control mats e-PLA and e- PLA CO 2 were developed in order to understand the effect of electrospinning and scCO2 impregnation, respectively, on PLA properties. Both strategies of incorporation of this active compound into PLA matrix resulted in different morphologies that influenced chemical and physical properties of these composites and in different release kinetics of CIN. The electrospinning and scCO2 impregnation processes and the presence of CIN altered PLA thermal and structural properties when compared to an extruded PLA material. The incorporation of CIN through scCO2 impregnation resulted in higher release rate and lower diffusion coefficients when compared to active electrospun mats with CIN incorporated during the electrospinning process.

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The knowledge of the biological properties of fruits and leaves of murta (Ugni molinae Turcz.) has been owned by native Chilean culture. The present study investigated the phenolic content, the antioxidant, antimicrobial and anti-tyrosinase activities of different murta fruit and leaves extracts to approach their uses on future food, pharmaceutical and cosmetic applications. Extractions of murta fruit and leaves were carried out under water, ethanol and ethanol 50%. Phenolic content of these extracts was measured through Folin Ciocalteu test and the antioxidant power by four different antioxidant systems (ORAC, FRAP, DPPH and TEAC assays) owing to elucidate the main mechanism of antioxidant. Some flavonoids, such as rutin, isoquercitrin and quercitrin hydrate were identified and quantified through HPLC analysis. Antimicrobial activity was determined measuring minimum inhibition concentration (MIC) and minimum bactericidal concentration (MBC) values against Escherichia coli and Listeria monocytogenes, and the effect of these extracts on L. monocytogenes was confirmed by flow cytometry. Highest contents of polyphenol compounds were obtained in hydroalcoholic extracts (28±1mggallicacid/g dry fruit, and 128±6mggallicacid/g dry leaves). The same trend was found for the values of biological properties: hydroalcoholic extracts showed the strongest activities. Leaves presented higher antioxidant, antimicrobial and anti-tyrosinase properties than murta fruit. Highest antioxidant activity values according to ORAC, FRAP, TEAC and DPPH were 80±8mgTrolox/g, 70±2mgTrolox/g, 87±8mgTrolox/g and 110±12mgTrolox/g, respectively, for murta fruit samples, and 280±10mgTrolox/g, 192±4mgTrolox/g, 286±13mgTrolox/g and 361±13mgTrolox/g, respectively, for murta leaves. These activities were confirmed by HPLC analysis that revealed highest presence of analyzed compounds on leaves hydroalcoholic extract. Regarding to antimicrobial analysis, hydroalcoholic leaves extract presented the highest activity presenting the lowest MIC value for L. monocytogenes (0.07mg/mL). This extract also performed the highest anti-tyrosinase activity (CE50 values of 1.6±0.3 (g/L) and 8.9±1.2 (g/L) for leaves and fruit, respectively).

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Electrospun nanofibers of poly (vinyl alcohol) (PV) were obtained to improve dispersion of cellulose nanocrystals (CNC) within hydrophobic biopolymeric matrices, such as poly(lactic acid) (PLA). Electrospun nanofibers (PV/CNC)n were successfully obtained with a final concentration of 23% (w/w) of CNC. Morphological, structural and thermal properties of developed CNC and electrospun nanofibers were characterized. X-ray diffraction and thermal analysis revealed that the crystallinity of PV was reduced by the electrospinning process, and the incorporation of CNC increased the thermal stability of biodegradable nanofibers. Interactions between CNC and PV polymer also enhanced the thermal stability of CNC and improved the dispersion of CNC within the PLA matrix. PLA materials with CNC lyophilized were also casted in order to compare the properties with materials based on CNC containing nanofibers. Nanofibers and CNC were incorporated into PLA at three concentrations: 0.5%, 1% and 3% (CNC respect to polymer weight) and nanocomposites were fully characterized. Overall, nanofibers containing CNC positively modified the physical properties of PLA materials, such as the crystallinity degree of PLA which was greatly enhanced. Specifically, materials with 1% nanofiber 1PLA(PV/CNC)n presented highest improvements related to mechanical and barrier properties; elongation at break was enhanced almost four times and the permeation of oxygen was reduced by approximately 30%.

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In this work, electrospun fibers of polyvinyl alcohol (PV) and starch (ST) were obtained to improve dispersion of cellulose nanocrystals (CNC) within a poly(lactic acid) (PLA) matrix with the aim of enhancing mechanical and barrier properties. The development and characterization of electrospun fibers with and without CNC, followed by their incorporation in PLA at three concentrations (0.5%, 1% and 3% with respect to CNC) were investigated. Morphological, structural, thermal, mechanical and barrier properties of these nanocomposites were studied. The purpose of this study was not only to compare the properties of PLA nanocomposites with CNC embedded into electrospun fibers and nanocomposites with freeze-dried CNC, but also to study the effect of electrospinning process and the incorporation of CNC on the PV and starch properties. SEM micrographs confirmed the homogenous dispersion of fibers through PLA matrix. X-ray analysis revealed that the electrospinning process decreased the crystallinity of PV and starch. The presence of CNC enhanced the thermal stability of electrospun fibers. Electrospun fibers showed an interesting nucleating effect since crystallinity of PLA was strongly increased. Nanocomposites with electrospun fibers containing CNC presented slightly higher flexibility and ductility without decreasing barrier properties.

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Fruits and vegetables are considered a good source of polyphenols and antioxidant capacities which are beneficial in protecting the human body against damage induced by reactive species. The objective of this work is to conduct an assessment of the polyphenol content and antioxidant activities of different fruit (kiwi, pear, green apple, raspberry, blackberry, strawberry and blueberry) and vegetable (pumpkin, green and red pepper) extracts using both chemical extraction and a modified in vitro digestive enzymatic extraction in order to compare results. Polyphenol content and antioxidant capacity of different fruits, vegetables and fruit juices were determined by Folin-Ciocalteu and FRAP methods, respectively. It was observed that polyphenol content expressed as gallic acid equivalents of extracts obtained with the two extraction methods was significantly (p<0.05) different (on average 310.3 and 231.8 mg per 100 g of fresh sample in enzymatic and methanolic extracts, respectively). Antioxidant capacity was also significantly (p<0.05) different in the extracts obtained by the two methods, with higher values in enzymatic extracts (1.91 mmol of Fe2+ per 100 g of fresh sample). Analyses of apple samples with and without skin also revealed important differences related to methodology and composition. Additionally, the original enzymatic extraction method was improved to avoid interferences caused by the presence of protein residues in the extract.

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Development of antioxidant and antimicrobial active food packaging materials based on biodegradable polymer and natural plant extracts has numerous advantages as reduction of synthetic additives into the food, reduction of plastic waste, and food protection against microorganisms and oxidation reactions. In this way, active films based on methylcellulose (MC) and maqui (Aristotelia chilensis) berry fruit extract, as a source of antioxidants agents, were studied. On the other hand, due to the high water affinity of MC, this polymer was firstly cross-linked with glutaraldehyde (GA) at different concentrations. The results showed that the addition of GA decreased water solubility, swelling, water vapor permeability of MC films, and the release of antioxidant substances from the active materials increased with the concentration of GA. Natural extract and active cross-linked films were characterized in order to obtain the optimal formulation with the highest antioxidant activity and the best physical properties for latter active food packaging application.

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