In the present study, a multilayer, high-barrier, thin blown film based on a polybutylene adipate terephthalate (PBAT) blend with polyhydroxyalkanoate (PHA), and composed of four layers including a cellulose nanocrystal (CNC) barrier layer and an electrospun poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) hot-tack layer, was characterized in terms of the surface roughness, surface tension, migration, mechanical and peel performance, barrier properties, and disintegration rate. The results showed that the film exhibited a smooth surface. The overall migration tests showed that the material is suitable to be used as a food contact layer. The addition of the CNC interlayer had a significant effect on the mechanical properties of the system, drastically reducing the elongation at break and, thus, the flexibility of the material. The film containing CNCs and electrospun PHBV hot-tack interlayers exhibited firm but not strong adhesion. However, the multilayer was a good barrier to water vapor (2.4 ± 0.1 × 10−12 kg·m−2·s−1·Pa−1), and especially to oxygen (0.5 ± 0.3 × 10−15 m3·m−2·s−1·Pa−1), the permeance of which was reduced by up to 90% when the CNC layer was added. The multilayer system disintegrated completely in 60 days. All in all, the multilayer system developed resulted in a fully compostable structure with significant potential for use in high-barrier food packaging applications.

This study reports on the development and characterization of organic recyclable high-oxygen-barrier multilayer films based on different commercial polyhydroxyalkanoate (PHA) materials, including a blend with commercial poly(butylene adipate-co-terephthalate) (PBAT), which contained an inner layer of cellulose nanocrystals (CNCs) and an electrospun hot-tack adhesive layer of poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) derived from cheese whey (CW). As a result, the full multilayer structures were made from bio-based and/or compostable materials. A characterization of the produced films was carried out in terms of morphological, optical, mechanical, and barrier properties with respect to water vapor, limonene, and oxygen. Results indicate that the multilayer films exhibited a good interlayer adhesion and contact transparency. The stiffness of the multilayers was generally improved upon incorporation of the CNC interlayer, whereas the enhanced elasticity of the blend was reduced to some extent in the multilayer with CNCs, but this was still much higher than for the neat PHAs. In terms of barrier properties, it was found that 1 µm of the CNC interlayer was able to reduce the oxygen permeance between 71% and 86%, while retaining the moisture and aroma barrier of the control materials.

One of the routes to minimize the environmental impact of plastics waste is the use of bio-sourced and biodegradable alternatives, particularly for packaging applications. Although Polyhydroxyalkanoates (PHA) are attractive candidates for food packaging, they have poor processability, particularly for extrusion film blowing. Thus, one relatively successful alternative has been blending PHA with a biodegradable polymer. This work proposes film blowing of a co-extruded Poly (hydroxybutyrate) (PHB) layer with a poly butylene adipateco-terephtalate (PBAT) layer to enhance bubble stability, mechanical and barrier properties. Co-extrusion is detailed, together with the different strategies followed to improve adhesion between film layers and the PHB content in the films. Films with thicknesses below 50 micron and elongation at break beyond 500% were consistently produced.

Active multilayer films based on polyhydroxyalkanoates (PHAs) with and without high barrier coatings of cellulose nanocrystals (CNCs) were herein successfully developed. To this end, an electrospun antimicrobial hot-tack layer made of poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) derived from cheese whey, a by-product from the dairy industry, was deposited on a previously manufactured blown film of commercial food contact PHA-based resin. A hybrid combination of oregano essential oil (OEO) and zinc oxide nanoparticles (ZnONPs) were incorporated during the electrospinning process into the PHBV nanofibers at 2.5 and 2.25 wt%, respectively, in order to provide antimicrobial properties. A barrier CNC coating was also applied by casting from an aqueous solution of nanocellulose at 2 wt% using a rod at 1m/min. The whole multilayer structure was thereafter assembled in a pilot roll-to-roll laminating system, where the blown PHA-based film was located as the outer layers while the electrospun antimicrobial hot-tack PHBV layer and the barrier CNC coating were placed as interlayers. The resultant multilayer films, having a final thickness in the 130–150 µm range, were characterized to ascertain their potential in biodegradable food packaging. The multilayers showed contact transparency, interlayer adhesion, improved barrier to water and limonene vapors, and intermediate mechanical performance. Moreover, the films presented high antimicrobial and antioxidant activities in both open and closed systems for up to 15 days. Finally, the food safety of the multilayers was assessed by migration and cytotoxicity tests, demonstrating that the films are safe to use in both alcoholic and acid food simulants and they are also not cytotoxic for Caco-2 cells.

The oxygen can have an adverse effect on the quality of some foods leading to a decrease in their shelf-life. Several approaches have been applied to remove the oxygen concentration in packed food; among them, oxygen scavengers have been widely used to preserve oxygen-sensitive foods. In the present study, an experimental set-up was designed to evaluate the effectiveness of oxygen scavengers, in removing oxygen from butter containers. Two types of oxygen absorbers adhesive labels and sachets and two caps with and without adjustable closure were tested. The plastic caps used in the study were characterized by differential scanning calorimetry and Fourier transform infrared spectroscopy. The oxygen concentration in the headspace of the containers was monitored using a gas analyser. The best results were achieved with the oxygen absorber sachets and using caps with adjustable closure. Under these conditions, the oxygen concentration inside the container remained below 3% during 150 h.

Studies on nanoparticles have focused the attention of the researchers because they can produce nanocomposites that exhibit unexpected hybrid properties. Polymeric materials are commonly used in food packaging, but from the standpoint of food safety, one of the main concerns on the use of these materials is the potential migration of low molecular substances from the packaging into the food. The key parameters of this phenomenon are the diffusion and partition coefficients. Studies on migration from food packaging with nanomaterials are very scarce. This study is focused on the determination of partition coefficients of different model migrants between the low-density polyethylene (LDPE) and polypropylene (PP) and between LDPE and nanocomposite polypropylene (naPP). The results show that the incorporation of nanoparticles in polypropylene increases the mass transport of model migrants from LDPE to naPP. This quantity of migrants absorbed into PP and naPP depends partially on the nature of the polymer and slightly on the chemical features of the migrant. Relation (RPP/naPP) between partition coefficientKLDPE/PPand partition coefficientKLDPE/naPPat 60°C and 80°C shows that only BHT at 60°C has aRPP/naPPless than 1. On the other hand, bisphenol A has the highestRPP/naPPwith approximately 50 times more.

New active films based on chitosan and polycaprolactone blends and containing α-tocopherol were designed for food packaging applications. Mechanical properties, stability against temperature and swelling degree in 50 % ethanol (v/v) were evaluated. Migration kinetics of α-tocopherol from the developed films into butter and food simulants [50 % ethanol (v/v), 95 % ethanol (v/v), and isooctane] at different temperatures were studied. α-Tocopherol was quantified in the food simulants by means of high performance liquid chromatography with diode-array detection at 292 nm. The proposed method exhibited a good sensitivity with a limit of detection of 0.1 mg/L. The kinetics release of α-tocopherol was characterized by determining the partition and the diffusion coefficients by using a mathematical modeling based on Fick’s Second Law. The diffusion coefficients obtained ranged between 1.03 × 10−13 and 2.24 × 10−12 cm2/s for 95 % ethanol (v/v) at 4 and 20 °C, respectively. Developed films maintained the antioxidant activity for more than 20 days.

The aim of this paper was to characterize chitosan samples from the shrimp shells for the later development of antimicrobial active systems. These systems include 100 % chitosan-based films obtained by casting, polyamide films with 5 and 10 % of chitosan obtained by extrusion and polyethylene/polyethylene terephthalate films with a coating of 0.6 % of chitosan. For that purpose, several analytical techniques including IR, 1H NMR, GPC, and microscopic techniques (scanning electron microscopy and transmission electron microscopy) were used. Within the studied samples, C1 showed the lowest DA and MW and consequently presented the most suitable properties for the development of an active packaging. Additionally, mechanical properties were performed. The effectiveness of the developed systems was evaluated by means of microbiological assays. The tested films showed antimicrobial capacity against coliform enterobacteria, mesophilic aerobic microorganism, and yeast and moulds.

The aim is to develop active packaging films containing natural antioxidants and to evaluate their capacity to enhance the oxidative stability of beef during refrigeration. The antioxidant activity of a natural extract obtained from a brewery residual waste was evaluated and compared with that of a commercial rosemary extract and two synthetic antioxidants (BHT and propyl gallate). Different concentrations of each antioxidant were also added directly to beef samples, resulting in a reduction in lipid oxidation of up to 70–80% relative to the control. Active antioxidant films coated with PVPP-WS extract reduced lipid oxidation by up to 80%, relative to the control, during cold storage. The use of active packaging films containing natural extracts could improve the oxidative stability of meat products and should therefore be of great interest in the food industry.

The aim of this study was to develop and evaluate the effectiveness of active packaging films produced with a natural extract obtained from a residual stream generated during the PVPP cleaning process in the brewing industry after a process of elimination of excess of haze active polyphenols present in beer. The thermal stability of the active phenolic compounds was first established at 100°C and 200°C and then incorporated into ethylene vinyl acetate (EVA) and low-density polyethylene (LDPE) films by extrusion. Migration, antimicrobial activity and lipid oxidation tests showed that EVA film was the most suitable for incorporating the natural extract. Finally, EVA film was spiked with 3% and 6% (w/w) of the natural extract or functionalized nanoclays (0.6%, 1.2% and 1.8%). Functionalized nanoclays were prepared by combining untreated montmorillonite and 20% of natural extract. The films spiked with the highest concentrations of extract or functionalized nanoclays provided the best results by retarding both the oxidation of beef samples by around 60% and S. aureus growth. The active films developed in the present study show promise for use in the food industry.Industrial relevanceThe new active packaging films developed in this study with a natural extract obtained from a brewery waste and functionalized nanoclays (prepared with natural extract) showed the capacity to enhance the oxidative stability of beef during refrigeration with respect to control films. The use of functionalized nanoclays improves the effectiveness of the active packaging and minimizes the amount of natural extract required. The use of these active packaging films containing bioactive compounds with both antioxidant and antimicrobial properties could extend the shelf life of minimally processed meat products and should therefore be of great interest in the food industry.

This paper reports the development of an extraction process that allows selective recovery of polyphenols from a brewery waste stream. The antioxidant activity of this extract (EC50 = 0.23–0.3 g/L) was very high, similar to that of butylated hydroxyanisole (BHA) and higher than that of other synthetic antioxidants such as butylated hydroxytoluene (BHT). Crude extracts exhibited a high level of antimicrobial activity against Gram-positive and Gram-negative bacteria, when applied at concentrations of 1% and 3% (w/v). The antioxidant and antimicrobial activities can probably be attributed to the major phenolic compounds, such as protocatechuic, caffeic, p-coumaric and ferulic acids and catechin. With this procedure, the waste polyphenols could be used as cheap source of natural compounds, with potential applications in the food and health sectors. Substitution of synthetic additives with safe and effective natural additives may be of further benefit to the food industry.

The main aims of this study were to determine the phenolic profile of a crude extract obtained (at pilot scale) from a brewery waste stream and to evaluate the antioxidant activity of the extract. The total phenolic content was determined by the Folin–Ciocalteu assay, which revealed that 50% of the extract comprised phenolic compounds. The polyphenols, identified and quantified by RP-HPLC–DAD and HPLC-ESI–TOF-MS, were mainly flavonoids (catechin, epicatechin, gallocatechin, epigallocatechin, quercetin) and phenolic acids (ferulic acid, p-coumaric acid, caffeic acid, protocatechuic acid). The crude extract displayed a high DPPH radical scavenging activity (0.18g/L), similar to that of BHA (0.248g/L) and higher than that of BHT (2.54g/L). All three tested products displayed a similar ability to decrease oxidative bleaching of β-carotene (antioxidant activity coefficient of 623.8 for the crude extract, 653.3 for BHA, 559.6 for BHT). This type of brewery waste stream may be a promising source of natural antioxidants to replace the synthetic antioxidants currently used in the food industry.

The brewery industry generates waste that could be used to yield a natural extract containing bioactive phenolic compounds. We compared two methods of purifying the crude extract—solid-phase extraction (SPE) and supercritical fluid extraction (SFE)—with the aim of improving the quality of the final extract for potential use as safe food additive, functional food ingredient, or nutraceutical. The predominant fractions yielded by SPE were the most active, and the fraction eluted with 30% (v/v) of methanol displayed the highest antioxidant activity (0.20 g L−1), similar to that of BHA. The most active fraction yielded by SFE (EC50 of 0.23 g L−1) was obtained under the following conditions: temperature 40°C, pressure 140 bar, extraction time 30 minutes, ethanol (6%) as a modifier, and modifier flow 0.2 mL min−1. Finally, we found that SFE is the most suitable procedure for purifying the crude extracts and improves the organoleptic characteristics of the product: the final extract was odourless, did not contain solvent residues, and was not strongly coloured. Therefore, natural extracts obtained from the residual stream and purified by SFE can be used as natural antioxidants with potential applications in the food, cosmetic, and pharmaceutical industries.

Natamycin is an antibiotic belonging to the group of polyene macrolides extensively employed as additive to prevent the microbial deterioration in food. The Annex III of the Directive 95/2/EC fixes in 1 mg/dm(2) the maximum level of the antifungal allowed in the final product.Reliable and sensitive methods for the analysis of natamycin are required to guarantee compliance with food legislation as well as to improve consumer protection.In the present paper, a simple and rapid high performance liquid chromatographic method with diode-array detection (HPLC-DAD) to determine natamycin in food samples was developed. Natamycin was extracted from food samples by using methanol acidified with acetic acid. The chromatographic separation was performed on a reversed-phase Kromasil ODS (08) (150 x 3.20 mm i.d., 5 mu m particle size) and the analysis was completed within 6 min. The method was validated in terms of linearity, limits of detection and quantification, repeatability and recovery. Satisfactory repeatability (R.S.D. (n = 10) < 4%, excellent sensitivity CLOD: 0.01 mu g/mL; LOQ: 0.05 mu g/mL) and appropriate recoveries were achieved.With the proposed method natamycin levels were determined in different food items. Data showed that two samples exceeded the limit established by the Annex III of the Directive 95/2/EC. Natamycin was also detected in samples in which its use is not allowed. The results were confirmed by LC-MS/MS using electrospray ionization (ESI) in positive mode. (C) 2013 Elsevier Ltd. All rights reserved.

This work was funded under the Project no. 95935 from FONCICYT C002-2008-1/ ALA – 127 249. The authors are grateful to the postdoctoral contract of Ana Sanches Silva in the frame of the Program “Science 2007” funded by “Fundacao para a Ciencia e para a Tecnologia”.

Nowadays, there is increasing interest in natural antioxidants from food by-products. Astaxanthin is a potent antioxidant and one of the major carotenoids in crustaceans and salmonids. An ultra-high pressure liquid chromatographic method was developed and validated for the determination of astaxanthin in shrimp by-products, and its migration from new packaging materials to food simulants was also studied. The method uses an UPLC® BEH guard-column (2.1 × 5 mm, 1.7 µm particle size) and an UPLC® BEH analytical column (2.1 × 50 mm, 1.7 µm particle size). Chromatographic separation was achieved using a programmed gradient mobile phase consisting of (A) acetonitrile-methanol (containing 0.05 m ammonium acetate)-dichloromethane (75:20:5, v/v/v) and (B) ultrapure water. This method was evaluated with respect to validation parameters such as linearity, precision, limit of detection, limit of quantification and recovery. Low-density polyethylene films were prepared with different amounts of the lipid fraction of fermented shrimp waste by extrusion, and migration was evaluated into food simulants (isooctane and ethanol 95%, v/v). Migration was not detected under the tested conditions.