Biodegradable Mono and Multilayer Materials with Antimicrobial Capacity Based on Circular Bioeconomy of Application Interest in Food Packaging

Tesis por compendio[ES] El envasado activo es una de las tecnologías emergentes más relevantes de la industria alimentaria. Su objetivo es interactuar con el espacio de cabeza del envase para controlar las reacciones enzimáticas, químicas, físicas y microbiológicas que deterioran los alimentos por medio de la absorción o liberación. La actual tesis doctoral trata originalmente del desarrollo y la caracterización de estructuras de envasado de alimentos activas y biodegradables mono y multicapa basadas en materiales de polihidroxialcanoatos (PHA) electroestirados derivados de estrategias de bioeconomía circular. Con el fin de dotar con propiedades activas los materiales de envasado, se incorporaron a los PHA aceites esenciales, extractos naturales, nanopartículas metálicas o combinaciones de los mismos mediante electrospinning de soluciones. Las fibras resultantes de PHA por electrospinning se recocieron para obtener monocapas continuas que, posteriormente, se combinaron con películas de polímeros biodegradables fundidas, sopladas o fundidas con disolventes y/o con revestimientos de barrera de nanocristales de celulosa bacteriana (CNC) para desarrollar novedosos sistemas multicapa con propiedades antimicrobianas y de barrera. Estos sistemas multicapas basados en PHA presentaron un buen rendimiento térmico y mecánico, así como altas propiedades de barrera a los vapores y gases. Las películas activas también mostraron mejores propiedades antioxidantes y una alta actividad antimicrobiana contra las bacterias transmitidas por los alimentos tanto en sistemas abiertos como, lo que es más importante, en sistemas cerrados, que pueden imitar las condiciones de envasado en casos reales. Por lo tanto, los materiales y prototipos desarrollados en este trabajo pueden ser muy prometedores como materiales de envasado, para constituir bandejas, flow packs y tapas, siendo completamente renovables y también biodegradables, con una potencial capacidad de aumentar tanto la calidad, como la seguridad de los productos alimenticios en el nuevo contexto de la Bioeconomía Circular.[CA] L'envasament actiu és una de les tecnologies emergents més rellevants de la indústria alimentària. El seu objectiu és interactuar amb l'espai de cap de l'envàs per controlar les reaccions enzimàtiques, químiques, físiques i microbiològiques que deterioren els aliments per mitjà de l'absorció o alliberament. L'actual tesi doctoral tracta originalment de el desenvolupament i la caracterització d'estructures d'envasat d'aliments actives i biodegradables mono i multicapa basades en materials de polihidroxialcanoatos (PHA) electroestirados derivats d'estratègies de bioeconomia circular. Per tal de dotar amb propietats actives dels materials d'envasat, es van incorporar als PHA olis essencials, extractes naturals, nanopartícules metàl·liques o combinacions dels mateixos mitjançant electrospinning de solucions. Les fibres resultants de PHA per electrospinning es recocieron per obtenir monocapes contínues que, posteriorment, es van combinar amb pel·lícules de polímers biodegradables foses, bufades o foses amb dissolvents i / o amb revestiments de barrera de nanocristalls de cel·lulosa bacteriana (CNC) per desenvolupar nous sistemes multicapa amb propietats antimicrobianes i de barrera. Aquests sistemes multicapes basats en PHA van presentar un bon rendiment tèrmic i mecànic, així com altes propietats de barrera als vapors i gasos. Les pel·lícules actives també van mostrar millors propietats antioxidants i una alta activitat antimicrobiana contra bacteris transmeses pels aliments tant en sistemes oberts com, el que és més important, en sistemes tancats, que poden imitar les condicions d'envasament en casos reals. Per tant, els materials i prototips desenvolupats poden ser molt prometedors com materials d'envasat, per constituir safates, flow packs i tapes, sent completament renovables i també biodegradables, amb la capacitat potencial final d'augmentar tant la qualitat, com la seguretat de els productes alimentaris en el nou context de l'Bioeconomia Circular.[EN] Active packaging is one of the most relevant emerging technologies in the food industry. It aims to interact with the packaging headspace to control the enzymatic, chemical, physical, and microbiological reactions that deteriorate food through scavenging or releasing means. The current PhD thesis originally deals with the development and characterization of mono and multilayer active and biodegradable food packaging structures based on electrospun polyhydroxyalkanoates (PHA) materials derived from circular bioeconomy strategies. In order to provide the packaging materials with active properties, essential oils, natural extracts, metallic nanoparticles or combinations thereof were incorporated into PHA by solution electrospinning. The resultant electrospun PHA mats were annealed to obtain continuous monolayers that were, thereafter, combined with cast-extruded, blown or solvent-casted biodegradable polymer films and/or barrier coatings of bacterial cellulose nanocrystals (CNCs) to develop novel multilayer systems with antimicrobial and barrier properties. These PHA-based multilayers systems presented good thermal and mechanical performance as well as high barrier properties to vapors and gases. The active films also showed improved antioxidant properties and high antimicrobial activity against food-borne bacteria in both open and, more importantly, closed systems, which can mimic real case use packaging conditions. Therefore, the here-developed materials and prototypes can be very promising as packaging materials, to constitute trays, flow packs and lids, being completely renewable and also biodegradable, with the final potential capacity to increase both quality and safety of food products in the new Circular Bioeconomy context.Al programa Santiago Grisolía de la Generalitat Valenciana (0001426013N810001A201) por concederme la beca Predoctoral. Al proyecto EU H2020 YPACK “High Performance Polyhydroxyalkanoates Based Packaging to Minimise Food Waste” (Grant agreement 773872) de la Comisión Europea. Al proyecto RTI2018-097249-B-C21 financiado por el Ministerio de Ciencia e Innovación de España. A la Unidad Asociada IATA-UJI en “Polymer Technology”.Figueroa López, KJ. (2021). Biodegradable Mono and Multilayer Materials with Antimicrobial Capacity Based on Circular Bioeconomy of Application Interest in Food Packaging [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/168439TESISCompendi

The impact of electrospun films of poly(epsilon-caprolactone) filled with nanostructured zeolite and silica microparticles on in vitro histamine formation by Staphylococcus aureus and Salmonella Paratyphi A

[EN] This research study originally reports the preparation and characterization of electrospun films based on poly(epsilon-caprolactone) (PCL) with high histamine-binding capacity. To this end, submicron PCL fibers filled with nanostructured zeolite or silica (SiO2) microparticles in the 5-20 wt% range were first prepared by solution electrospinning. The resultant electrospun composite fiber mats were thereafter thermally post-treated at 55 degrees C to successfully develop contact-transparent films with reduced porosity and improved mechanical strength. The capacity of the developed composite films to entrap histamine was evaluated in vitro by the culture media method using Staphylococcus aureus (S. aureus) and Salmonella Paratyphi A (S. Paratyphi A) foodborne bacteria. Both electrospun zeolite- and SiO2-containing PCL films exhibited high histamine-binding capacity, being more effective for S. aureus. The histamine entrapment performance was significantly higher for the PCL films filled with zeolite due to the enhanced porous structure and more optimal adsorption selectivity of this inorganic filler. The here-developed electrospun composite films can be applied as novel active-scavenging packaging materials to entrap heat-stable histamine and other biogenic amines released from fish and fishery products.This research was funded by the Spanish Ministry of Science, Innovation, and Universities (MICIU) program number AGL2015-63855-C2-1-R and by the EU H2020 YPACK project (reference number 773872). The authors also thank the Republic of Turkey Ministry of Agriculture and Forestry General Directorate of Agricultural Research and Policies (TAGEM) and Central Fisheries Research Institute SUMAE) for funding support through the projects TAGEM/HSGYAD/14/A05/P05/70 and TAGEM/HSGYAD/17/A03/P05/133. Figueroa Lopez is a recipient of a Santiago Grisolia (GRISOLIAP/2017/101) grant of the Generalitat Valenciana (GVA) and Torres-Giner is on a Juan de la Cierva-Incorporacion contract (IJCI-2016-29675) from MICIU.Alp-Erbay, E.; Figueroa-López, KJ.; Lagaron, JM.; Çaglak, E.; Torres-Giner, S. (2019). The impact of electrospun films of poly(epsilon-caprolactone) filled with nanostructured zeolite and silica microparticles on in vitro histamine formation by Staphylococcus aureus and Salmonella Paratyphi A. Food Packaging and Shelf Life. 22:1-13. https://doi.org/10.1016/j.fpsl.2019.100414S11322Alp Erbay, E., Dağtekin, B. B. (Gözü), Türe, M., Yeşilsu, A. F., & Torres-Giner, S. (2017). Quality improvement of rainbow trout fillets by whey protein isolate coatings containing electrospun poly(ε-caprolactone) nanofibers with Urtica dioica L. extract during storage. LWT, 78, 340-351. doi:10.1016/j.lwt.2017.01.002Alp-Erbay, E., Yeşi̇lsu, A. F., & Türe, M. (2019). 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Foodborne Pathogens and Disease, 9(2), 108-112. doi:10.1089/fpd.2011.098

Caracterización óptica y estructural de nanopartículas de Allium sativum L. impregnadas en lomo de bovino

En el trabajo se determinaron las características ópticas y estructurales de nanopartículas de polvo de ajo (Allium sativum L.), obtenidas por reducción y selección de tamaño, para comparación con muestras de polvo de ajo comercial. El tamaño de partícula se determinó empleando microscopía electrónica de transmisión (TEM) y las caracterizaciones óptica y estructural se realizaron, respectivamente, por espec-troscopia infrarroja transformada de Fourier (FTIR) y difracción de rayos X (DRX). Para determinar el efecto de las nanopartículas de polvo de ajo cuando fueron aplicadas sobre trozos de lomo (Longissimus dorsi) de bovino se utilizó la técnica de fluorescencia. Los tamaños de las partículas del polvo sometido a reducción y selección de tamaño presentaron valores entre 50 y 100 nm y las de polvo de ajo normal entre 400 y 500 nm. En los espectros de FTIR se observaron los principales grupos funcionales y los difracto-gramas de rayos X permitieron concluir que se trata de materiales amorfos. Por su tamaño más reducido, las nanopartículas migran más rápido al interior del músculo del bovino que las micropartículas, lo que permite una mejor absorción y aprovechamiento de sus componentes y se constituye en un resultado innovadores en el campo de la ciencia de los alimentos.To determine the optical and structural characteristics of garlic powder, garlic powder nanoparticles were obtained by size reduction and selection methods and their optical and structural characteristics were determined. The optical and structural response between commercial garlic powders and powders obtained by size reduction operations was compared. The particle size was determined using transmission electron microscopy (TEM) images; the optical characterization was determined using Fourier transform infrared spectroscopy (FTIR) spectra and the structural characterization was made using X-ray diffraction (XRD). Bovine loin (Longissimus dorsi) samples were impregnated with garlic powder nanoparticles and the tissue was characterized by fluorescence technique. Powders obtained with size reduction and selection methods presented sizes values between 50 and 100 nm, while the normal garlic powder between 400 and 500 nm. FTIR spectra showed the presence of the main functional groups and X -ray diffractograms allowed to infer that the structure of garlic as an amorphous material

Effect of different essential oils on the properties of edible coatings based on yam (dioscorea rotundata l.) starch and its application in strawberry (fragaria vesca l.) preservation

Every year the world loses about 50% of fruits and vegetables post-harvest and in the supply chain. The use of biodegradable coatings and films with antioxidant properties has been considered an excellent alternative to extend the shelf life of food. Therefore, the objective of this work was to develop a coating based on yam (Dioscorea rotundata L.) starch-containing lime, fennel, and lavender essential oils to extend the shelf life of strawberries (Fragaria vesca l.). The tensile properties, barrier properties (water vapour permeability (WVP) and oxygen permeability (OP)), moisture content, water-solubility, absorption capacity, water contact angle, optical properties, the antioxidant activity of the resultant starch-based coatings were evaluated. After that, the active properties of the coatings were assessed on strawberries inoculated with Aspergillus niger during 14 days of storage at 25 °C. The results showed that the incorporation of essential oils improved the elongation and WVP and provided antioxidant capacity and antimicrobial activity in the films. In particular, the essential oil of lime showed higher antioxidant activity. This fact caused the unwanted modification of other properties, such as the decrease in tensile strength, elastic modulus and increase in OP. The present study revealed the potential use of lime, fennel, and lavender essential oils incorporated into a polymeric yam starch matrix to produce biodegradable active films (antioxidant and antimicrobial). Obtained films showed to be a viable alternative to increase the shelf life of strawberries and protect them against Aspergillus niger