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Expanded polystyrene will account for 5.3% of total global plastic production in 2021 and is widely used for food packaging due to its excellent moisture resistance and thermal insulation. However, some of these packages are often used only once before being discarded, generating large amounts of environmentally harmful plastic waste. A very attractive alternative to the conventional methods used for polymer processing is the use of supercritical carbon dioxide (scCO 2 ) since it has mass-transfer properties adapted to the foam morphology, generating different path lengths for the diffusion of active compounds within its structure and can dissolve a wide range of organic molecules under supercritical conditions. The objective of this research was to evaluate the effect of operational variables on the process of caffeic acid (CA) impregnation and subsequent foaming of polylactic acid (PLA) as well as two PLA/poly(butylene-co-terephthalate-adipate) (PBAT) blends using scCO 2 . The results showed an increase in the degree of crystallinity of the CA-impregnated samples due to the nucleation effect of the active compound. On the other hand, SEM micrographs of both films and foams showed significant differences due to the presence of PBAT and its low miscibility with PLA. Finally, the results obtained in this work contribute to the knowledge of the important parameters to consider for the implementation of the impregnation and foaming process of PLA and PLA/PBAT blends with potential use in food packaging.

In the last decade, among the emerging technologies in the area of bioplastics, additive manufacturing (AM), commonly referred to as 3D printing, stands out. This technology has gained great interest in the development of new products, mainly due to its capability to easily produce customized and low-cost plastic products. This work aims to evaluate the effect of supercritical foaming of 3D-printed parts based on a commercial PLA matrix loaded with calcium carbonate, for single-use sustainable food contact materials. 3D-printed PLA/CaCO 3 parts were obtained by 3D printing with a 20% and 80% infill, and two infill patterns, rectilinear and triangular, were set for each of the infill percentages selected. Supercritical fluid foaming of PLA/CaCO 3 composite printed parts was performed using a pressure of 25 MPa, a temperature of 130 °C for 23 min, with a fast depressurization rate (1 s). Closed-cell foams were achieved and the presence of CaCO 3 did not influence the surface of the foams or the cell walls, and no agglomerations were observed. Foam samples with 80% infill showed subtle temperature fluctuations, and thermogravimetric analysis showed that samples were thermally stable up to ~300 °C, while the maximum degradation temperature was around 365 °C. Finally, tensile test analysis showed that for lower infill contents, the foams showed lower mechanical performance, while the 80% infill and triangular pattern produced foams with good mechanical performance. These results emphasize the interest in using the supercritical CO 2 process to easily produce foams from 3D-printed parts. These materials represent a sustainable alternative for replacing non-biodegradable materials such as Expanded Polystyrene, and they are a promising option for use in many industrial applications, such as contact materials.

Compounds derived from essential oils have been used in active packaging, but their volatility and degradability negatively affect stability and leads to high release rates. The present study aimed to develop PLA bionanocomposite foams loaded with carvacrol cocrystal by supercritical CO 2 and its release into a food simulant for control release in food packaging. For this purpose, 4,4'-bipyridine was used as coformer and carvacrol as active agent. Cocrystallized closed cell foams were obtained using supercritical CO 2 and were characterized in terms of their physicochemical and mechanical properties, and release kinetics to a D1 simulant were evaluated as well as the antioxidant ability. A better overall mechanical behavior due to the nanoclay promoting a higher interfacial adhesion with the polymeric matrix was revealed. A higher incorporation of carvacrol was observed in samples with higher C30B content. The incorporated cocrystals showed a decrease of one order of magnitude in the estimated effective diffusion coefficient of carvacrol and showed antioxidant activity. These results suggest that the nanocomposite foam containing carvacrol-based cocrystals could be used in active packaging systems with controlled release characteristics, especially with highly volatile compounds, and can be proposed for other fields such as biomedical applications., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023. Published by Elsevier B.V.)

β-cyclodextrin and allyl isothiocyanate inclusion complexes (β-CD:AITC) have been proposed for developing fresh fruit and vegetable packaging materials. Therefore, the aim of this research was to develop active materials based on poly(lactic acid) (PLA) loaded with β-CD:AITC and to assess changes in the material properties during the release of AITC to food simulants. PLA films with 0, 5 and 10 wt.% β-CD:AITC were developed by extrusion. Surface properties were determined from contact angle measurements. Films were immersed in water, aqueous and fatty simulants to assess the absorption capacity and the change in the thermal properties. Moreover, the release of AITC in both simulants was evaluated by UV-spectroscopy and kinetic parameters were determined by data modeling. Results showed that a higher concentration of β-CD:AITC increased the absorption of aqueous simulant of films, favoring the plasticization of PLA. However, the incorporation of β-CD:AITC also avoided the swelling of PLA in fatty simulant. These effects and complex relationships between the polymer, inclusion complexes and food simulant explained the non-systematic behavior in the diffusion coefficient. However, the lower partition coefficient and higher percentage of released AITC to the fatty simulant suggested the potential of these materials for high-fat fruit and vegetable active packaging applications.

Among the most promising synthetic biopolymers to replace conventional plastics in numerous applications is MaterBi ® (MB), a commercial biodegradable polymer based on modified starch and synthetic polymers. Actually, MB has important commercial applications as it shows interesting mechanical properties, thermal stability, processability and biodegradability. On the other hand, research has also focused on the incorporation of natural, efficient and low-cost active compounds into various materials with the aim of incorporating antimicrobial and/or antioxidant capacities into matrix polymers to extend the shelf life of foods. Among these is ellagic acid (EA), a polyphenolic compound abundant in some fruits, nuts and seeds, but also in agroforestry and industrial residues, which seems to be a promising biomolecule with interesting biological activities, including antioxidant activity, antibacterial activity and UV-barrier properties. The objective of this research is to develop a film based on commercial biopolymer Mater-Bi ® (MB) EF51L, incorporating active coating from chitosan with a natural active compound (EA) at two concentrations (2.5 and 5 wt.%). The formulations obtained complete characterization and were carried out in order to evaluate whether the incorporation of the coating significantly affects thermal, mechanical, structural, water-vapor barrier and disintegration properties. From the results, FTIR analysis yielded identification, through characteristic peaks, that the type of MB used is constituted by three polymers, namely PLA, TPS and PBAT. With respect to the mechanical properties, the values of tensile modulus and tensile strength of the MB-CHI film were between 15 and 23% lower than the values obtained for the MB film. The addition of 2.5 wt.% EA to the CHI layer did not generate changes in the mechanical properties of the system, whereas a 5 wt.% increase in ellagic acid improved the mechanical properties of the CHI film through the addition of natural phenolic compounds at high concentrations. Finally, the disintegration process was mainly affected by the PBAT biopolymer, causing the material to not disintegrate within the times indicated by ISO 20200.

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.

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.

Betalains are bioactive compounds with remarkable functional and nutritional activities for health and food preservation and attractiveness. Nevertheless, they are highly sensitive to external factors, such as oxygen presence, light, and high temperatures. Therefore, the search for new structures, polymeric matrices, and efficient methods of encapsulation of these compounds is of great interest to increase their addition to food products. In this work, betalains were extracted from red beetroot. Betacyanin and betaxanthin contents were quantified. Subsequently, these compounds were successfully encapsulated into the core of coaxial electrosprayed capsules composed of hydroxypropyl methylcellulose (HPMC) and gelatin (G). The effect of incorporating the carbohydrate and the protein both in the core or shell structures was studied to elucidate the best composition for betalain protection. Morphological, optical, and structural properties were analyzed to understand the effect of the incorporation of the bioactive compounds in the morphology, color, and chemical interactions between components of resulting electrosprayed capsules. The results of the thermogravimetric and encapsulation efficiency analysis coincided that the incorporation of beetroot extract in G in the core and HPMC in the shell resulted in the structure with greater betalain protection. The effectiveness of the core/shell structure was confirmed for future food applications.

This article proposes a foaming method using supercritical carbon dioxide (scCO 2 ) to obtain compostable bionanocomposite foams based on PLA and organoclay (C30B) where this bionanocomposite was fabricated by a previous hot melt extrusion step. Neat PLA films and PLA/C30B films (1, 2, and 3 wt.%) were obtained by using a melt extrusion process followed by a film forming process obtaining films with thicknesses between 500 and 600 μm. Films were further processed into foams in a high-pressure cell with scCO 2 under constant conditions of pressure (25 MPa) and temperature (130 °C) for 30 min. Bionanocomposite PLA foams evidenced a closed cell and uniform cell structure; however, neat PLA presented a poor cell structure and thick cell walls. The thermal stability was significantly enhanced in the bionanocomposite foam samples by the good dispersion of nanoclays due to scCO 2 , as demonstrated by X-ray diffraction analysis. The bionanocomposite foams showed improved overall mechanical performance due to well-dispersed nanoclays promoting increased interfacial adhesion with the polymeric matrix. The water uptake behavior of bionanocomposite foams showed that they practically did not absorb water during the first week of immersion in water. Finally, PLA foams were disintegrated under standard composting conditions at higher rates than PLA films, showing their sustainable character. Thus, PLA bionanocomposite foams obtained by batch supercritical foaming seem to be a sustainable option to replace non-biodegradable expanded polystyrene, and they represent a promising alternative to be considered in applications such as food packaging and other products.

Background: Allyl isothiocyanate is an excellent antimicrobial compound that has been applied in the development of active food packaging materials in the last years. However, the high volatility of this compound could prevent a lasting effect over time. In order to avoid this problem, cyclodextrin inclusion complexes have been proposed as an alternative, being beta-cyclodextrin (β-CD) as the main candidate. In addition, β-CD could act as a relative humidity-responsive nanoparticle. In this regard, the aim of this study was to develop inclusion complexes based on β-CD and AITC as relative humidity-responsive agents, which can be used in the design of active food packaging materials. Methods: Two different β-CD:AITC inclusion complexes (2:1 and 1:1 molar ratios) were obtained by the co-precipitation method. Entrapment efficiency was determined by gas chromatography, while inclusion complexes were characterized through thermal, structural, and physicochemical techniques. Antifungal capacity of inclusion complexes was determined in a headspace system. Furthermore, the AITC release from inclusion complexes to headspace at different percentages of relative humidity was evaluated by gas chromatography, and this behavior was related with molecular dynamic studies. Key Findings and Conclusions: The entrapment efficiency of inclusion complexes was over to 60%. Two coexisting structures were proposed for inclusion complexes through spectroscopic analyses and molecular dynamic simulation. The water sorption capacity of inclusion complexes depended on relative humidity, and they exhibited a strong fungicide activity against Botrytis cinerea . Furthermore, the AITC release to headspace occurred in three stages, which were related with changes in β-CD conformational structure by water sorption and the presence of the different coexisting structures. In addition, a strong influence of relative humidity on AITC release was evidenced. These findings demonstrate that β-CD:AITC inclusion complexes could be used as potential antifungal agents for the design of food packaging materials, whose activity would be able to respond to relative humidity changes., Competing Interests: The authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest., (Copyright © 2022 Muñoz-Shugulí, Rodríguez-Mercado, Mascayano, Herrera, Bruna, Guarda and Galotto.)

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.

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.

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., (© 2021 Institute of Food Technologists®.)

Core/shell electrospun mats based on cellulose acetate (CA) and polycaprolactone (PCL) were developed as novel active materials for releasing quercetin (Quer) and curcumin (Cur). The effect of polymeric uniaxial and coaxial electrospun systems and the chemical structures of Quer and Cur on the structural, thermal, and mass transfer properties of the developed mats were investigated. Release modelling indicated that the diffusion of the active agents from the uniaxial PCL fibers was highly dependent on the type of food simulant. Higher diffusion coefficients were obtained for both active agents in acid food simulant due to the higher swelling of the electrospun mats. In addition, CA/PCL coaxial structures slowed down the diffusion of both active agents into both food simulants. CA increased the retention of the active compounds in the polymer structure, resulting in partition coefficients values higher than the values obtained for uniaxial active PCL mats., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

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.

Poly (lactic acid)/lignin nanocomposites (PLA/Lig-Np) containing cinnamaldehyde (Ci) were obtained by a combination of melt extrusion and supercritical impregnation process. In this work, Ci impregnation tests were carried out in a high-pressure cell at 40 °C for 3 h using 12 MPa and 1 MPa min -1 of depressurization rate, obtaining impregnation yields ranging from 5.7 to 10.8% w/w. Thermal, mechanical and colorimetric properties of the developed films were affected by the incorporation of lignin nanoparticles and the active compound, obtaining biodegradable plastic materials with a strong UV-light barrier property compared to PLA films. In addition, disintegrability tests under composting conditions confirmed the biodegradable character of nanocomposites developed. On day 23, a disintegration percentage greater than 90% was determined for all bionanocomposites. Finally, to establish the possible toxicity effect of the nanocomposites obtained, studies in vivo were performed in normal rats. Toxicity studies showed normal blood parameters after a single dose of nanocomposites. PLA/Ci/Lig-Np bionanocomposite films could be potentially applied to design biodegradable UV-light barrier materials for food packaging and biomedical applications., Competing Interests: Declaration of competing interest There are no conflicts of interest to declare., (Copyright © 2020 Elsevier B.V. All rights reserved.)

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., (© 2020 Institute of Food Technologists®.)

A new active coating was developed by using Cucumis metuliferus fruit extract as antioxidant additive with the aim of obtaining an easy way to functionalize low-density polyethylene (LDPE) films for food packaging applications. Thus, an extraction protocol was first optimized to determine the total phenolic compounds and the antioxidant activity of CM. The aqueous CM antioxidant extract was then incorporated into cellulose acetate (CA) film-forming solution in different concentrations (1, 3 and 5 wt.%) to be further coated in corona-treated LDPE to obtain LDPE/CA-CM bilayer systems. CA and CA-CM film-forming solutions were successfully coated onto the surface of LDPE, showing good adhesion in the final bilayer structure. The optical, microstructural, thermal, mechanical and oxygen barrier performance, as well as the antioxidant activity, were evaluated. The active coating casted onto the LDPE film did not affect the high transparency of LDPE and improved the oxygen barrier performance. The antioxidant effectiveness of bilayer packaging was confirmed by release studies of Cucumis metuliferus from the cellulose acetate layer to a fatty food simulant. Finally, the LDPE/CA-CM active materials were also tested for their application in minimally processed fruits, and they demonstrated their ability to reduce the oxidation process of fresh cut apples. Thus, the obtained results suggest that CA-CM-based coating can be used to easily introduce active functionality to typically used LDPE at industrial level and enhance its oxygen barrier, without affecting the high transparency, revealing their potential application in the active food packaging sector to extend the shelf-life of packaged food by prevention of lipid oxidation of fatty food or by prevention fruit browning.

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., Competing Interests: The authors declare no conflicts of interest.

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.

The search for and synthesis of new antimicrobial nanostructures is important to reduce microbial incidence that induces infectious diseases and to aid in the antibiotic resistance crisis, which are two of the most pressing issues in global public health. In this work, novel, hollow, calcined titanium dioxide nanospheres (CSTiO 2 ) were successfully synthesized for the first time through the combination of electrospinning and atomic layer deposition techniques. Poly(vinylpyrrolidone) (PVP) electrosprayed spherical particles were double-coated with alumina and titanium dioxide, and after a calcination process, hollow nanospheres were obtained with a radius of approximately 345 nm and shell thickness of 17 nm. The structural characterization was performed using electron microscopy, and X-ray diffraction and small-angle X-ray diffraction evidenced an anatase titanium dioxide crystalline structure. Thermogravimetric analysis and Fourier-transform infrared spectroscopy studies demonstrated the absence of polymer residue after the calcination process. The antimicrobial properties of the developed CSTiO 2 hollow nanospheres were evaluated against different bacteria, including resistant E. coli and S. aureus strains, and when compared to commercial TiO 2 nanoparticles, CSTiO 2 nanospheres exhibited superior performance. In addition, the positive effect of UV irradiation on the antimicrobial activity was demonstrated.

Inclusion complexes based on β-cyclodextrin (β-CD) and antimicrobial compounds, were prepared by co-precipitation method, and characterized by entrapment efficiency (EE), thermal analysis, X-ray diffraction, 1 H NMR spectroscopy, and water sorption. In addition, experiments associated to evaluate the effect of relative humidity on the release of active compounds and antifungal tests were performed. The analysis evidenced the encapsulation of active compounds into the β-CD structure with EE of 91 ± 4.1% and 66 ± 2.1% for β-CD/cinnamaldehyde and β-CD/eugenol complexes, respectively. Additionally, high relative humidities favored the release of active compounds from inclusion complexes. On the other hand, inclusion complexes were able to control the growth of B. cinerea, which was evidenced by a reduction of its mycelialradial growth. Finally, specific interactions between the active compounds and β-CD were evaluated through molecular dynamics simulation techniques. According to the obtained results, these complexes could be applied as additives in the design of antifungal packaging., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

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/CIN imp ). 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.

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., Competing Interests: The authors declare no conflicts of interest.

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 (CE 50 values of 1.6±0.3 (g/L) and 8.9±1.2 (g/L) for leaves and fruit, respectively)., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

The release of microencapsulated natural antimicrobial (AM) agents (thymol and carvacrol) from two encapsulating matrixes [maltodextrin (MD) and soy protein (SP)] were evaluated for possible use in food packaging coatings. Microcapsules were prepared by oil-in-water (O/W) emulsions at different concentrations (10, 20% for MD and 2, 5% for SP). High encapsulation efficiency ranged from 96 to 99.95% for MD and 93.1 to 100% for SP, with average microcapsule diameters that ranged from 17 to 27.5 and 18.8 to 38 µm, respectively. The release rate with 20% MD-thymol [20MD-T] was faster than with 10% MD-thymol [10MD-T]. Similar results were obtained for carvacrol with the same concentration of MD. Korsmeyer-Peppas and Weibull mathematical models were successfully fitted to the release of the AM agents, describing the Fickian diffusion release of the components. Different release rates were obtained as a function of the chemical nature of the encapsulation material and its concentration., Competing Interests: Compliance with ethical standardsThe authors declare no conflict of interest.

Supercritical impregnation was used to incorporate a natural compound with antibacterial activity into biopolymer-based films to develop active food packaging materials. Impregnation tests were carried out under two pressure conditions (9 and 12MPa), and three depressurization rates (0.1, 1 and 10MPamin -1 ) in a high-pressure cell at a constant temperature equal to 40°C. Cinnamaldehyde (Ci), a natural compound with proven antimicrobial activity, was successfully incorporated into poly(lactic acid) films (PLA) using supercritical carbon dioxide (scCO 2 ), with impregnation yields ranging from 8 to 13% w/w. Higher pressure and slower depressurization rate seem to favor the Ci impregnation. The incorporation of Ci improved thermal, structural and mechanical properties of the PLA films. Impregnated films were more flexible, less brittle and more resistant materials than neat PLA films. The tested samples showed strong antibacterial activity against the selected microorganisms. In summary, this study provides an innovative route to the development of antibacterial biodegradable materials, which could be used in a wide range of applications of active food packaging., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

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%.

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.

An important issue in food technology is that antimicrobial compounds can be used for various applications, such as the development of antimicrobial active packaging materials. Yet most antimicrobial compounds are volatile and require protection. In the present study, the inclusion complexes of 2-nonanone (2-NN) with β-cyclodextrin (β-CD), were prepared by a co-precipitation method. Entrapment efficiency (EE), thermal analysis (DSC and TGA), X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FT-IR), sorption isotherms and antifungal activity were evaluated for the characterization of the inclusion complex (β-CD:2-NN). A higher EE was obtained (34.8%) for the inclusion complex 1:0.5 than for other molar rates. Both DSC and TGA of the inclusion complexes showed the presence of endothermic peaks between 80 °C and 150 °C, attributed to a complexation phenomenon. Antimicrobial tests for mycelial growth reduction under atmospheric conditions proved the fungistatic behaviour of the inclusion complexes against Botrytis cinerea., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

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., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

Antioxidant biocomposites have been successfully developed from cellulose acetate, eco-friendly triethyl citrate plasticizer and onion extract as a source of natural antioxidants. First, an onion extraction process was optimized to obtain the extract with highest antioxidant power. Extracts under absolute ethanol and ethanol 85% were the extracts with the highest antioxidant activity, which were the characterized through different methods, DPPH (2,2-diphenyl-1-picrylhydrazyl) and ABTS (2,2'-azinobis(3-ethylbenzothiazoline-6-sulphonate)), that measure radical scavenger activity, and polyphenolic and flavonoid content. Afterwards, the extract was incorporated in cellulose acetate as polymer matrix owing to develop an active material intended to oxidative sensitive food products packaging. Different concentrations of onion extract and plasticizer were statistically studied by using response surface methodology in order to analyze the influence of both factors on the release of active compounds and therefore the antioxidant activity of these materials.

Cellulose acetate (CA)/copper montmorillonite modified (MtCu(2+)) antimicrobial nanocomposites for food packaging containing 1, 3 and 5 wt.% nanoparticles were prepared by solution casting technique. X-ray diffraction (XRD) and transmission electron microscopy revealed the existence of intercalated and no intercalated clay form in the CA matrix. The thermal stability of the MtCu(2+)/CA nanocomposites was measured by TGA and DSC, which indicated that the nanocomposites were less thermally stable in comparison to CA pure. Mechanical testing of material did not show differences when MtCu(2+) was added in CA. On the other hand, antimicrobial effect was observed for nanocomposites films, obtaining a 98% reduction against Escherichia coli., (Copyright © 2013 Elsevier Ltd. All rights reserved.)

Nanocomposites based on biopolymers have been recognised as potential materials for the development of new ecofriendly food packaging. In addition, if these materials incorporate active substances in their structure, the potential applications are much higher. Therefore, this work was oriented to develop nanocomposites with antimicrobial activity based on cellulose acetate (CA), a commercial organoclay Cloisite30B (C30B), thymol (T) as natural antimicrobial component and tri-ethyl citrate (TEC) as plasticiser. Nanocomposites were prepared by a solvent casting method and consisted of 5% (w/w) of C30B, 5% (w/w) of TEC and variable content of T (0%, 0.5% and 2% w/w). To evaluate the effect of C30B into the CA matrix, CA films without this organoclay but with T were also prepared. All nanocomposites showed the intercalation of CA into the organoclay structure; furthermore this intercalation was favoured when 2% (w/w) of T was added to the nanocomposite. In spite of the observed intercalation, the presence of C30B inside the CA matrices increased the opacity of the films significantly. On the other hand, T showed a plasticiser effect on the thermal properties of CA nanocomposites decreasing glass transition, melting temperature and melting enthalpy. The presence of T in CA nanocomposites also allowed the control de Listeria innocua growth when these materials were placed in contact with this Gram-positive bacterium. Interestingly, antimicrobial activity was increased with the presence of C30B. Finally, studies on T release showed that the clay structure inside the CA matrix did not affect its release rate; however, this nanofiller affected the partition coefficient KP/FS which was higher to CA nanocomposites films than in CA films without organoclay. The results obtained in the present study are really promising to be applied in the manufacture of food packaging materials.

Five types of macroalgae from the southern hemisphere were analysed for the presence of β-1,3/1,6-glucan and its immunostimulant properties. We were able to extract soluble β-1,3/1,6-D-glucan from Durvillaea antarctica (Chamisso) Hariot (DA). The morphology of the brown algae influenced extraction, and the highest percentage of β-glucan was found in the fronds. The content of β-glucan in the stipes and holdfast was on average 33% and <5%, respectively, of that in the fronds. A simple laboratory extraction process was developed. A highly pure water-soluble polysaccharide, mainly composed of glucose residues, was obtained with a dominant average molecular weight of 6.9 kDa. NMR spectroscopy confirmed the polysaccharide structure to be of β-1,3/1,6-glucan type, comprising a β-1,3-glucan backbone and 21% degree of branching of β-1,6-glucan side chains. Mouse cells were exposed to four DA extract concentrations in water (50, 100, 250 and 500 μg/mL) and no adverse effects on survival were noted. Remarkably, the β-glucan induced a 16.9% increase in activated CD19+ B lymphocytes compared with the control sample. The optimal concentration for maximum activity was 100 μg DA extract/mL., (Copyright © 2012 Elsevier Ltd. All rights reserved.)

The aim of the present study was to determine the antimicrobial (AM) properties of plastic flexible films with a coating of microcapsules containing carvacrol and thymol as natural AM agents. Microencapsulation of these agents enables their controlled release and leads to the destruction (or growth inhibition) of a broad spectrum of microorganisms such as, Escherichia coli O157:H7, Staphylococcus aureus, Listeria innocua, Saccharomyces cerevisiae and Aspergillus niger. It was found that the studied AM agents are strong inhibitors to the growth of mycelium, but they were not effective against spore germination of mold. Thymol (T) and carvacrol (C) showed a significant AM activity against the studied microorganisms, with minimal inhibitory concentrations (MIC) of 125-250 ppm and 75-375 ppm for thymol and carvacrol respectively. The synergistic effect of combinations of thymol and carvacrol was also studied and it was found that the highest synergism was achieved at a concentration of 50% T and 50% C. The release of the AM agents was carried out at 4°C during 28 days. The concentration of the microencapsulated AM agents showed a range of zones of inhibition of 4.3-11.3mm for the microorganisms at 10% of thymol and 10% of carvacrol. At these concentrations the release of the AM agents (within 48 h) was greater than required for the most resistant microorganism (E .coli O157:H7), as reflected by the relatively large zone of inhibition. The results of the present study confirm the suitability of using microencapsulated thymol and carvacrol incorporated in polymer films for AM food packaging., (Copyright © 2011 Elsevier B.V. All rights reserved.)

The dietary intake of total arsenic (tAs), inorganic arsenic (iAs) and total mercury (tHg) in lunch and breakfast servings provided by the Chilean School Meal Program (SMP) was estimated, using the duplicate-portion variant of the total diet study. Lunch and breakfast samples were collected from 65 schools throughout the country in 2006. The population sample was a group of girls and boys between 6 and 18 years old. The tAs concentration was measured via hydride-generation atomic absorption spectrometry. The total mercury concentration was measured via cold-vapor atomic absorption spectroscopy. The estimated iAs intake was 12.5% (5.4 μg/day) of the Provisional tolerable daily intake (PTDI) as proposed by the FAO/WHO, and the tHg intake was 13.2% (1.9 μg/day) of the PTDI as proposed by the FAO/WHO. It was therefore concluded that tAs, iAs and tHg intake from food provided by the SMP do not pose risks to student health.

The effect of high-pressure processing on 2 plastic food packaging films, a biopolymer (PLASiOx/PLA) and a synthetic polymer (PET-AlOx), was studied. Samples in direct contact with olive oil, as a fatty food simulant, and distilled water, as an aqueous simulant, were subjected to a pressure of 500MPa for 15 min at 50 degrees C. The mechanical, thermal, and gas barrier properties of both films were evaluated after the high-pressure processing (HPP) and compared to control samples that have not undergone this treatment. Significant changes in all properties were observed in both films after the HPP treatment and in contact with the food simulants. In both films an induced crystallization was noticed. In the PLASiOx/PLA film the changes were larger when in contact with water that probably acted as a plasticizer. In the PET-AlOx film the changes in properties were attributed to the formation of pinholes and cracks during the HPP treatment. In this film, most of the properties changed more in the presence of oil as the food simulant.