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Plastic recycling is the main solution to reduce the plastic waste. High-density polyethylene has not been recycled yet successfully as food contact material due to the amount of chemicals present in post-consumer material together with its high chemical sorption capacity. The migration of two post-consumer recycled HDPE milk bottles were studied to both 50 % ethanol as food simulant and real food (one type skimmed milk and two plant base beverages (soy milk and horchata). Firstly, a headspace-solid phase extraction-gas chromatography mass spectrometry method was developed and optimized to analyze these milky samples. After exposure, 53 compounds were identified and among them several additives, NIAS such as 2,5-cyclohexadiene-1,4-dione, 2,6-bis(1,1-dimethylethyl), 2,4-di-tert-butylphenol and 7,9-di-tert-butyl-1-oxaspiro(4,5)deca-6,9-diene-2,8-dione, degradation products of antioxidant compounds as well as several residues from cleaning products, detergents and flavoring agents were found. Finally, the risk assessment was applied and it was found that five compounds did not comply after migration to 50 % ethanol.

Biopolymers based on polylactic acid (PLA) and starch have numerous advantages, such as coming from renewable sources or being compostable, though they can have deficiencies in mechanical properties, and for this reason, polyester resins are occasionally added to them in order to improve their properties. In this work, migration from a PLA sample and from another starch-based biopolymer to three different food simulants was studied. Attention was focused on the determination of oligomers. The analysis was first performed by ultraperformance liquid chromatography quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF–MS), which allowed the identification of the oligomers present in migration. Then, the samples were analyzed by two ambient desorption/ionization techniques directly coupled to mass spectrometry (ADI), direct analysis in real-time coupled to standardized voltage and pressure (DART-MS) and atmospheric pressure solids analysis probe (ASAP-MS). These methodologies were able to detect simultaneously the main oligomers migrants and their adducts in a very rapid and effective way. Nineteen different polyester oligomers, fourteen linear and five cyclic, composed of different combinations of adipic acid [AA], propylene glycol [PG], dipropylene glycol [DPG], 2,2-dibutyl-1,3-propanediol [DBPG], or isobutanol [i-BuOH] were detected in migration samples from PLA. In migration samples from starch-based biopolymer, fourteen oligomers from poly(butylene adipate co-terephthalate) polyester (PBAT) were identified, twelve cyclic and two linear. The results from ADI techniques showed that they are a very promising alternative tool to assess the safety and legal compliance of food packaging materials. Graphical abstract Supplementary Information The online version contains supplementary material available at 10.1007/s00216-021-03755-0.

The characterization and quantification of phenolic compounds in bearberry leaves were performed using hyphenated ion mobility spectroscopy (IMS) and a quadrupole time-of-flight mass spectrometer. A higher identification confidence level was obtained by comparing the measured collision cross section (TWCCSN2) with predicted values using a machine learning algorithm. A total of 88 compounds were identified, including 14 arbutin derivatives, 33 hydrolyzable tannins, 6 flavanols, 26 flavonols, 9 saccharide derivatives, and glycosidic compounds. Those most reliably reproduced in all samples were quantified against respective standards. Arbutin (47-107 mg/g), 1,2,3,4,6-pentagalloylglucose (6.6-12.9 mg/g), and quercetin 3-galactoside/quercetin 3-glucoside (2.7-5.7 mg/g) were the most abundant phenolic components in the leaves. Quinic acid and ellagic acid were also detected at relatively high concentrations. The antioxidant activity of the most abundant compounds was evaluated. A critical view of the advantages and limitations of traveling wave IMS and CCS for the discovery of natural products is given.

Recycling of polymers is one of the alternatives to reduce the impact of polymers presence on the environmental. However, the contaminants, defined as non-intentionally added substances, present in recycled material may migrate into food and also change its molecular structure. This work addresses the extractability/migration of contaminants from polypropylene (PP) samples into food simulants and the influence of these contaminants on the molecular structure of recycled PP. For this PP was contaminated with several substances to simulate a “worst-case” scenario and, then it was submitted to a recycling process. Extractability tests were performed by solid-phase microextraction and gas chromatography coupled to mass spectroscopy both to evaluate the presence of contaminants in the PP samples and their ability to migrate in food simulants. Additionally, molecular changes of the PP samples were evaluated by oscillatory rheometry. After washing and extrusion of the PP samples the extractability results showed considerable reductions of migrations in the food simulants and indicated, in some cases, compliance with regulations for using recycled polymer in contact with food. The residual contaminants were present in the polymer, the high temperatures and shear rates play an important role in molecular changes. Finally, the results highlight the importance of the use of rheological measurements to detect the influence of contaminants in recycled materials. Their presence result in material with different molar mass, that may be applied in different market applications.

This research aimed to study the migration of mineral oil aromatic hydrocarbons (MOAH) from primary carton packages to dry foods, using 16 aromatic hydrocarbons as model substances, covering a wide range of molecular masses and chemical structures. Migration experiments were performed using modified polyphenylene oxide as a food simulant and couscous and polenta as dry foods. The migration tests were carried out to simulate storage at room temperature for long periods and in hot food containers as the worst scenario. Multivariate analysis algorithms were applied to correlate and group the migration of model substances, and a partial least squares regression (PLSR) model was built to predict the worst-case migration. The results showed strong correlations in the migration patterns of the model substances, based on their volatility, food matrix, migration time and temperature. Different behaviour between the migration of the most volatile and the heaviest model substances was observed.

There are numerous approaches and methodologies for assessing the identity and quantities of non-intentionally added substances (NIAS) in food contact materials (FCMs). They can give different results and it can be difficult to make meaningful comparisons. The initial approach was to attempt to prepare a prescriptive methodology but as this proved impossible; this paper develops guidelines that need to be taken into consideration when assessing NIAS. Different approaches to analysing NIAS in FCMs are reviewed and compared. The approaches for preparing the sample for analysis, recommended procedures for screening, identification, and quantification of NIAS as well as the reporting requirements are outlined. Different analytical equipment and procedures are compared. Limitations of today's capabilities are raised along with some research needs.

This article studies the migration of MOAH from hot melt adhesives used in multilayer laminates into food simulants. First, the initial concentration of a group of compounds selected as MOAH markers in several adhesives was determined by headspace solid phase microextraction coupled to gas chromatography mass spectrometry (HS-SPME-GC-MS), using the previously optimised method. Then, the migration of the MOAH fraction and MOAH markers from the laminates was studied. The MOAH fraction was analysed by gas chromatography with flame ionisation detection (GC-FID), and the MOAH markers were analysed by HS-SPME-GC-MS. Twelve MOAH markers were detected, and their initial concentrations were between 0.46 and 33.8 μg g-1. Only eight were identified after migration, ranging between 0.62 and 21.33 μg dm-2, with a migration percentage of 12–75%. The fraction of MOAH that migrated eluted mainly in the C16-C25 range and reached concentrations of 19.65 μg dm-2 from the laminate.

Although most new biomaterials for food industry applications are labelled ‘100% natural fabrication’ and ‘chemical-free’, certain compounds may migrate from those materials to the food, compromis- ing the organoleptic characteristics and safety of the product. In this work, the degree of compound migration from dishes made with four different biomaterials: bamboo, palm leaf, wood and wheat pulp was investigated. Migration tests were carried out using three food simulants, 10% ethanol (sim- ulant A), 3% acetic acid (simulant B), and 95% ethanol (simulant D2). Unequivocal identification of non-intentionally added substances (NIAS) is challenging even when using high-resolution mass spectrometry techniques however, a total of 25 different non-volatile compounds from the migration tests were identified and quantified using Ultra-high performance liquid chromatography coupled to ion mobility quadrupole time-of-flight mass spectrometry (UPLC-IMS-MS). In the bamboo samples three oligomers, cyclic diethylene glycol adipate, 3,6,9,16,19,22-hexaoxabicyclo[22.3.1]-octacosa-1(28),24,26- triene-2,10,15,23-tetrone and 1,4,7,14,17,20-hexaoxacyclohexacosane-8,13,21,26-tetrone exceeded the specified limits of migration.

Food packaging is of high societal value because it conserves and protects food, makes food transportable and conveys information to consumers. It is also relevant for marketing, which is of economic significance. Other types of food contact articles, such as storage containers, processing equipment and filling lines, are also important for food production and food supply. Food contact articles are made up of one or multiple different food contact materials and consist of food contact chemicals. However, food contact chemicals transfer from all types of food contact materials and articles into food and, consequently, are taken up by humans. Here we highlight topics of concern based on scientific findings showing that food contact materials and articles are a relevant exposure pathway for known hazardous substances as well as for a plethora of toxicologically uncharacterized chemicals, both intentionally and non-intentionally added. We describe areas of certainty, like the fact that chemicals migrate from food contact articles into food, and uncertainty, for example unidentified chemicals migrating into food. Current safety assessment of food contact chemicals is ineffective at protecting human health. In addition, society is striving for waste reduction with a focus on food packaging. As a result, solutions are being developed toward reuse, recycling or alternative (non-plastic) materials. However, the critical aspect of chemical safety is often ignored. Developing solutions for improving the safety of food contact chemicals and for tackling the circular economy must include current scientific knowledge. This cannot be done in isolation but must include all relevant experts and stakeholders. Therefore, we provide an overview of areas of concern and related activities that will improve the safety of food contact articles and support a circular economy. Our aim is to initiate a broader discussion involving scientists with relevant expertise but not currently working on food contact materials, and decision makers and influencers addressing single-use food packaging due to environmental concerns. Ultimately, we aim to support science-based decision making in the interest of improving public health. Notably, reducing exposure to hazardous food contact chemicals contributes to the prevention of associated chronic diseases in the human population.

The rapid growth of polymer technology in the field of food contact materials (FCMs) needs to be supported by continuous improvement in material testing, in order to ensure the safety of foodstuff. In this work, a range of different starch-based biopolymer samples, in the shape of pellets and retail samples (cups and dishes) were studied. The optimized extraction process was performed on three different pellet shapes: pellets with no modification (spherical), pellets shattered under high pressure (lentils), and pellets cryogenically ground (powder). The analysis of unknown volatile and semi-volatile compounds was carried out by gas chromatography-mass spectrometry, using both electron ionization with a single quadrupole mass analyzer (GC-EI-MS), and atmospheric pressure gas chromatography with a quadrupole/time of flight mass analyzer (APGC-Q/ToF). The identification process was implemented using the latest advances in the understanding of APGC ionization pathways. Chemical migration was also assessed on prototype samples using the food simulants: ethanol 10% v/v, acetic acid 3% w/V, ethanol 95% v/v, isooctane, and vegetable oil. Each migration test was performed three consecutive times, as recommended for materials intended for repeated use.

Food packaging is tailored to keep food fresh by increasing shelf life and preventing microbial deterioration. However, traditional food packaging is commonly made from non-degradable polymers without antimicrobial properties and that pose an environmental threat if not disposed properly. To address this issue, here we describe the preparation of cellulose nanofibril (CNF) films and hydrogels with antimicrobial activity against common foodborne pathogens such as verotoxigenic E. coli, L. monocytogenes and S. Typhimurium. Furthermore, two grades of negatively charged CNFs with different fibrillation degrees were modified with ethyl lauroyl arginate (LAE), which is an antimicrobial agent. CNF films were able to bind LAE molecules up to a maximum concentration of 145–160 ppm. LAE–CNF biocomposite films exerted a bactericidal activity against a major foodborne pathogen present in ready-to-eat food (L. monocytogenes) even at 1% LAE. Our work describes a novel biopolymer-based strategy that overcomes the current hurdles with LAE incorporation into packaging materials, offering a green and antimicrobial alternative for packaging of ready-to-eat (RTE) meat products.

Polylactic acid (PLA) is a biopolymer commonly used in food packaging due to its good characteristics, similar to PET. To evaluate the safety of this material, the analysis of the non-intentionally added substances (NIAS) is required. Oligomers are NIAS and their behavior needs a deep study, especially if they migrate to the food. In this work, the analysis of the polymer and the migration to food simulants was carried out. A total dissolution/precipitation procedure was applied to PLA pellets and films, using dichloromethane and ethanol as solvent and antisolvent system respectively. The migration tests were carried out in three liquid simulants to mimic any kind of food. Since oligomers are not present in the positive list of the Directive 10/2011/EC, their concentration must be below the 0.01 mg/kg of food. UPLC-QTOF-MS, with and without ion mobility (IM), was used for the analysis. Thirty-nine different PLA oligomers made of repeated monomer units of [LA] (C3H4O2) and with different structures were identified. They corresponded to cyclic oligomers with [LA]n structure and two groups of linear oligomers, one with an hydroxyl group, OH–[LA]n–H, and the other one with an ethoxy group, CH3–CH2–O–[LA]n–H. Cyclic oligomers only appeared in the material and were not present in migration solutions. Linear oligomers HO–[LA]n–H were already present in the pellets/film and they migrated in a higher extension to aqueous food simulants (EtOH 10% and AcH 3%). However, linear oligomers CH3–CH2–O–[LA]n–H were not present initially in the pellets/film, but were detected in migration to simulants with ethanol content, EtOH 95% and EtOH 10%. Furthermore, 5 cyclic polyester oligomers were identified in migration. Ethanol 95% and ethanol 10% migration solutions were also analyzed by scanning electron microscopy (SEM), and the presence of microstructures that could be attributed to the oligomers migration was found. They could be seen as microplastics.

Widespread use of plastics poses a serious environmental hazard to our planet and should be substituted by eco-friendly and biodegradable alternatives, simultaneously reducing waste of perishable food products and the risk of transmission of pathogenic microbes. In our study, we describe how the water solubility of the antimicrobial surfactant ethyl lauroyl arginate (LAE) can be reduced through complexation with a Keggin-type polyoxometalate (POM), K8[SiW11O39]. The POM-LAE complex, LAE7K[SiW11O39], was effective against Listeria monocytogenes (L. monocytogenes) and Escherichia coli (E. coli) with minimal inhibitory concentrations (MICs) of 32 and 64 μg/mL, respectively, with the important finding that the concentrations of LAE required to inhibit bacterial growth were as much as two times lower in the POM-LAE complex, compared with LAE on its own. In addition, our results demonstrate that POM-LAE is both an effective inhibitor of biofilm formation and is also able to destroy pre-formed biofilms of L. monocytogenes and E. coli at MIC concentrations. Further, POM-LAE was incorporated into carboxymethyl cellulose (CMC) films that were able to reduce 7–8 log (CFU/mL) of L. monocytogenes at concentrations of 5–10% POM-LAE. In vivo assays of the POM-LAE-CMC films with cured ham prevented initialk bacterial growth with a 0.77 log significative reduction in bacterial counts. Overall, this work provides new alternatives for the development of antimicrobial biodegradable films for ready-to-eat (RTE) foods prone to contamination with pathogenic bacteria, such as L. monocytogenes, while also circumventing practical issues related to the incorporation of LAE into active packaging films., This work was supported by the Spanish Ministerio de Ciencia e Innovación (RTI2018-097805-B-I00 and PID2019-109333RB-I00), the Gobierno de Aragón (Project LMP49-18) and the Centre for the Development of Industrial Technology (1061/2020). N.G. acknowledges a fellowship from the Universidad de Zaragoza and Université de Pau et des Pays de l’Adour.

[EN] The EFSA Panel on Food Contact Materials, Enzymes and Processing Aids (CEP) assessed the safety of the recycling process ISAP Packaging (EU register number RECYC218), which uses the Starlinger deCON technology. The input material is hot washed and dried poly(ethylene terephthalate) (PET) flakes originating from collected post-consumer PET containers, e.g. bottles, including no more than 5% PET from non-food consumer applications. The flakes are preheated before being submitted to solid-state polycondensation (SSP) in a reactor at high temperature under vacuum and (sic) The process may be operated with more than one SSP reactor (normally four). Having examined the challenge test provided, the Panel concluded that the preheating (step 2) and the decontamination in the (sic) SSP reactor (step 3) are critical in determining the decontamination efficiency of the process. The operating parameters to control the performance of these critical steps are temperature, pressure, residence time and (sic) It was demonstrated that this recycling process is able to ensure a level of migration of potential unknown contaminants into food below the conservatively modelled migration of 0.1 mu g/kg food. Therefore, the Panel concluded that the recycled PET obtained from this process is not considered to be of safety concern, when used at up to 100% for the manufacture of materials and articles for contact with all types of foodstuffs for long-term storage at room temperature, with or without hotfill. The final articles made of this recycled PET are not intended to be used in microwave or conventional ovens and such uses are not covered by this evaluation. (C) 2021 European Food Safety Authority. EFSA Journal published by John Wiley and Sons Ltd on behalf of European Food Safety Authority

Four commercially available silicone cupcake molds have been studied. An evaluation of the post-cure treatment applied to the silicone molds was carried out and the loss of volatile organic compounds after cure treatment was quantified. The two higher quality molds showed losses at the 0.5% (w/w) (recommended by BfR standard), while the two lower quality molds exceeded this limit. The migration studies were carried out using Tenax® as a solid food simulant. The volatile compounds that migrate were identified and quantified using SPME-GC-MS. Up to fourteen silicone oligomers were quantified. When the molds were subjected to post-cure treatment, none of them exceeded the global migration of 10 mg/dm2; while those lower quality molds showed migrations higher than 10 mg/dm2, so their use in contact with food is not recommended.

An exhaustive migration study of eight corks, made of ethylene–vinyl acetate, was carried out to identify any non-volatile and volatile compounds using an untargeted approach. The challenge associated with the structural elucidation of unknowns was undertaken using both ultra-high-performance liquid chromatography coupled to an ion-mobility separation quadrupole-time of flight mass spectrometer and gas chromatography mass spectrometry. A total of fifty compounds were observed to migrate from the corks, and among these additives such as antioxidants (Butyl 4-hydroxybenzoate, Irganox 1010, Irganox 1075, Irgafos 168 and BHT) or lubricants (EBO and octadecanamide, N,N'-1,2-ethanediylbis-) were identified. A high proportion (84%) of the detected compounds was non-intentionally added substances (NIAS), and included several cyclic oligomers with different chain sequences. NIAS, such as 2,6-bis(1,1-dimethylethyl)-4-ethyl and 7,9-ditert-butyl-1-oxaspiro[4.5]deca-6,9-diene-2,8-dione, break-down products, including hexa-, hepta- and nonadecanamide, N,N'-1,2-ethanediylbis-, and oxidation products were also identified. One cork was found to be unsuitable for use as a food contact material.

The aim of this work was to select and identify the best markers of aromatic hydrocarbon mineral oil (MOAH) in food packaging. For this purpose, a series of mineral oils was initially analysed. Polycyclic Aromatic Hydrocarbons (PAHs) and the alkylated isomers of Methylnaphthalene (MNS), Diisopropylnaphtalene (DIPNs), Dibenzothiophenes (DBTS), Methyldibenzothiophene (MDBTs), Dimethyldibenzothiophenes (DMDBTs) and Benzonaphthiophenes (BNTS) were then explored. Their presence was confirmed by direct analysis of several mineral oils by Atmospheric Solids Analysis Probe Quadrupole-Time of Flight Mass Spectrometry (ASAP-QTOF-MS). Atmospheric Pressure Gas Chromatography Quadrupole-Time of Flight Mass Spectrometry (APGC-QTOF-MS) was used to confirm the markers in different samples of oils, recycled PET (rPET), recycled cardboard and packaging of couscous and semolina to confirm the contamination. 27 markers were found in the mineral oil samples, 22 of them in rPET, 8 in recycled board and no MOAH were found in packaging of couscous and semolina.

The electrospun nanosystems containing poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) and 1 wt% Fe doped ZnO nanoparticles (NPs) (with the content of dopant in the range of 0–1 wt% Fe) deposited onto polylactic acid (PLA) film were prepared for food packaging application. They were investigated by scanning electron microscopy (SEM), energy dispersive X-ray (EDX), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), antimicrobial analysis, and X-ray photoelectron spectrometry (XPS) techniques. Migration studies conducted in acetic acid 3% (wt/wt) and ethanol 10% (v/v) food simulants as well as by the use of treated ashes with 3% HNO3 solution reveal that the migration of Zn and Fe falls into the specific limits imposed by the legislation in force. Results indicated that the PLA/PHBV/ZnO:Fex electrospun nanosystems exhibit excellent antibacterial activity against the Pseudomonas aeruginosa (ATCC-27853) due to the generation of a larger amount of perhydroxyl (¿OOH) radicals as assessed using electron para-magnetic resonance (EPR) spectroscopy coupled with a spin trapping method. © 2021 by the authors. Licensee MDPI, Basel, Switzerland.

Ion mobility time-of-flight mass spectrometry has been used for the identification the PA 6 and PA 66 oligomers through their accurate m/z, CCS values and fragmentation pattern. An extraction method for the oligomers from sunflower oil, cooked beans, soup and whole milk has been developed with recoveries ranging from 87 to 102 %.

Nowadays, polypropylene is one of the most common polymers used in the food packaging industry due to its good functionality and relatively low cost. Nevertheless, usage of plastic disposable packaging can be a generator of plastic pollution having negative environmental effects. A feasible solution for this issue would be to recycle. The polypropylene samples were submitted to two processes, forced contamination, and recycling, and they were analyzed by solid-phase microextraction gas chromatograph-olfactometry-mass spectrometry. 45 different volatile compounds were identified and 9 of them presented distinct odoriferous activities. Among them, two important markers were detected: diethyl phthalate (probably coming from the catalyst of PP polymerization, intentionally added substance (IAS)), and glycerine (a marker of non-intentionally added substances (NIAS)).

Fresh chicken is a potential source of human infection due to its high microbial load, making the issues regarding its microbiological safety, especially the control of Campylobacter spp., of paramount relevance. Pinosylvin has recently proved effective against this major food pathogen. In this work, we evaluated the efficacy of absorbent pads containing pinosylvin (PS) inclusion complexes (ICs) for the control of fresh chicken meat microbial contamination, focusing on its anti-Campylobacter activity. Coated pads were evaluated in vitro against C. jejuni, followed by in vivo testing in chicken exudates and meat, assessing their anti-Campylobacter activity as well as their efficacy in inhibiting poultry microbiota. Pads exhibited a bactericidal activity in liquid medium at a concentration of 0.08 mg/cm2. At 4 °C, pads with 0.4 mg PS/cm2 exhibited anti-Campylobacter activity in chicken fillets and exudates. Regarding spoilage bacteria, active coated pads were not able to reduce pseudomonads but caused reductions in LAB, psychrotrophs and total viable counts. The present work demonstrates that absorbent pads coated with pinosylvin inclusion complexes possess an efficient antimicrobial activity not only against C. jejuni but also against chicken spoilage bacteria, enabling the use of these active pads to control microbial growth in packaged chicken meat.

Polyurethane adhesives are used to bond agglomerated cork and natural disk cork to produce cork stoppers that are used in champagne bottles. These adhesives are manufactured by reacting polyols with an excess of diisocyanates. Isocyanates are highly reactive compounds that have a propensity to form non-intentionally added substances (NIAS) in the end product. In this work, ion mobility-time of flight-mass spectrometry was used to elucidate such NIAS, through the comparison of accurate mass spectra with the fragmentation patterns of proposed candidates. Twelve neo-formed compounds, including amines, amides and urethanes, resulting from the reaction of isocyanates with acetic acid and ethanol used as food simulants, were identified. Additionally, markers from champagne vs. champagne after its exposure to the adhesive were investigated using the supervised multivariate analysis method of Orthogonal Projection to Latent Structures – Discriminant Analysis. Four neo-formed compounds, resulting from the reaction of diisocyanates with malic acid or tartaric acid contained in the champagne, were identified for the first time in this work. All of the compounds identified were subsequently quantified using ultra-high pressure liquid chromatography coupled to a triple quadrupole mass spectrometer. Limits of detection were below 5 μg/kg in the food simulants and below 30 μg/kg in champagne samples. Migration levels ranged from 70 to 721 μg/kg, with most of them exceeding the specific migration limit established for Cramer class III compound (90 μg/kg).

The present work reports an experimental study on the optimization of phenolic compounds extraction from Citrus ✕ paradisi peels and the development of active packaging. Response surface methodology (RSM) was applied to investigate the effect of microwave-assisted extraction (MAE) for the recovery of total phenolic compounds (TPC). The TPC in the optimized extract were 31.10 mg gallic acid equivalent/100 g of dry weight (mg GAE/100 g dw) with strong antioxidant capacity. The bioactive compounds in the optimized extract were determined by ultrahigh performance liquid chromatography coupled to quadrupole time-of-flight with high energy mass spectrometry (UPLC-QTOF-MSE). Forty-five compounds were detected and qualified. The optimized extract obtained by MAE was used as an active antioxidant in multilayer food packaging films. The multilayer low-density polyethylene (LDPE)/polyethylene terephthalate (PET) containing 10% of MAE optimized extract provided the most antioxidant power acting as a free radical scavenger.

Oligomers are potential migrants from polymers or biopolymers intended to food packaging and they have to be under control. In order to comply with European regulation 10/2011, their concentration in migration must be below 0.01 μg g-1. In this work, fabric phase sorptive extraction (FPSE) was explored as an effective method for extraction and pre-concentration of oligomers migrated from a blend PLA-polyester material. Both food simulant B (3% acetic acid) and juice, as real food, were used for migration experiments. The parameters of FPSE were optimized and the analysis was done by UHPLC-QTOF and UHPLC-QqQ. A total of 21 oligomers were identified, 9 of them coming from PLA and 12 oligomers from the polyester part. These oligomers were formed by adipic acid (AA), phthalic acid (PA) and/or butanediol (BD), ten were cyclic and 11 were linear molecules. Using the optimized FPSE procedure in 3% acetic acid as food simulant, it was possible to identify 3 new compounds that were not detected by direct injection of the simulant into UHPLC-QTOF. In addition, 2 extra compounds, cyclic PA-BD4-AA3 and cyclic PA2-BD3-AA, were only identified in juice samples after FPSE extraction. Besides, in order to quantify the compounds identified, an isolation procedure for PLA oligomers was carried out. Two oligomers were isolated: cyclic (LA)6 and linear HO-(LA)4-H, both with a purity higher than 90% (LA: lactic acid). The highest concentration value was found for the cyclic oligomer [AA-BD]2, that showed 22.63 μg g-1 in 3% acetic acid and 19.64 μg g-1 in juice. The concentration of the total amount of remaining oligomers was below 7.56 μg g-1 in 3% acetic acid as well as in juice.

Antimicrobial active packaging has emerged as an effective technology to reduce microbial growth in food products increasing both their shelf-life and microbial safety for the consumer while maintaining their quality and sensorial properties. In the last years, a great effort has been made to develop more efficient, long-lasting and eco-friendly antimicrobial materials by improving the performance of the incorporated antimicrobial substances. With this purpose, more effective antimicrobial compounds of natural origin such as bacteriocins, bacteriophages and essential oils have been preferred over synthetic ones and new encapsulation strategies such as emulsions, core-shell nanofibres, cyclodextrins and liposomes among others, have been applied in order to protect these antimicrobials from degradation or volatilization while trying to enable a more controlled release and sustained antimicrobial action. On that account, this article provides an overview of the types of antimicrobials agents used and the most recent trends on the strategies used to encapsulate the antimicrobial agents for their stable inclusion in the packaging materials. Moreover, a thorough discussion regarding the benefits of each encapsulation technology as well as their application in food products is presented.

New bamboo-based biopolymers are used as food packaging materials, but it must be evaluated to ensure consumers safety. In this study, migration from a commercial bamboo-based biopolymer to ethanol 10% (v/v), acetic acid 3% (w/v) and ethanol 95% (v/v) was studied. The migrants were determined from three different perspectives. Volatile and semi-volatile compounds were analyzed by gas chromatography-mass spectrometry (GC-MS). Twenty-five compounds were detected. In addition, a number of phytosterols were detected in ethanol 95%. Non-volatile compounds were identified and quantified by ultra-performance liquid chromatography coupled to time-of-flight mass spectrometry (UPLC-Q/ToF). Twelve non-volatile compounds were detected in migration solutions, mainly melamine and its derivatives, coming from polymer resins present in the biopolymer. Melamine migration was higher than 50 mg/Kg in the third sequential migration test. Finally, the migration samples were analyzed by DART-SVP (direct analysis in real time coupled to standardized voltage and pressure). This methodology was able to detect simultaneously the main volatile and non-volatile migrants and their adducts in a very rapid and effective way and is shown as a promising tool to test the safety and legal compliance of food packaging materials.

Artificial insemination is common practice in mass livestock farming. Recently, it was shown that chemicals leaching from multilayer plastic bags affect the fertility of boars, although common quality tests did not show any impact on the sperm. It is not clear whether this incidence was a single case or whether it could be a systematic problem. Therefore, we studied six multilayer plastic bags. A total of 49 compounds were found, but most of them were at very low intensity. Nonylphenols in the range of 19-99 μg/g plastic were found. Migration tests using water and 10% ethanol as simulants, to mimic the behavior of semen with the extender, were performed. The most interesting migrants in terms of potential reprotoxicity were identified as nonylphenols. The identification in depth demonstrated the presence of 10 isomers of nonylphenol with a total concentration range between 16 to 58 μg/Kg simulant, among other migrants at lower concentration. The influence of these nonylphenols and their maximum tolerable concentration in direct contact with semen from boars was studied. Motility, viability, mitochondrial activity and acrosomes reacted were significantly affected at 10 mg/Kg of nonylphenols in contact with the sperm, but in vitro penetration rate was significantly decreased with only 2 mg/Kg. Insight into the mode of action is also provided.

A novel and fast salting out liquid-liquid extraction method was developed for simultaneous determination of food additives with different polarities in juices. Chromatographic separation was achieved in less than 6 min using Acquity UPLC BEH C 18 (100 mm × 2.1 mm d.i. × 1.7 µm) column with ammonium acetate with 0.01% of trifluoroacetic acid as eluent A and acetonitrile as eluent B at a flow rate of 0.2 mL min−1. The main factors affecting the extraction efficiency were optimized. The method was validated applying accuracy profile based on total error. The extraction recoveries ranged from 84.97 to 122%. Relative standard deviation ranged from 1.24 to 7.99% for intraday assay and from 1.69 to 9.16% for intermediate precision. The limits of detection for five food additives were from 0.3 to 1.42 µg mL−1. The method was successfully applied to 47 samples of juices from nine brands.

Multilayer materials used in food packaging are commonly manufactured with a polyurethane adhesive layer in its structure that may contain cyclic esters oligomers as potential migrants. However, little is known about their toxicity. In this work, two cyclic esters of polyurethane are evaluated in migration from 20 multilayer packaging samples. They were composed by adipic acid (AA), diethylene glycol (DEG) and isophthalic acid (IPA) and their structure was AA-DEG and AA-DEG-IPA-DEG. The concentration of these compounds in migration exceeded the maximum level established by Regulation EU/10/2011 (10 ng g−1). Bioaccessibility of both compounds was evaluated by studying gastric and intestinal digestion. The studies showed that the concentration of the compounds decreased during digestion and that their hydrolysed molecules increased. Furthermore, endocrine activity in vitro assays were performed. A weak androgen receptor antagonism was identified, whereas no arylhydrocarbon receptor activity or binding to the thyroid hormone transport protein was found.

En este trabajo presentamos un método sencillo y rápido para confirmar la contaminación por aceites minerales (MOH) de distintos tipos de muestras mediante extracción por SPE y determinación por Cromatografía de Gases con Detector de masas.

Aim: The objective of the present study was to investigate in vitro anticoccidial effect of olive pulp (Olea europaea L var. Chemlal) extract on the destruction of Eimeria spp. oocysts isolated from infected chickens naturally. Materials and methods: The olive pulp (OP) powder was stirred manually in aqueous ethanol in preparation for extraction using the microwave-assisted extraction system. The identification of the phenolic compounds was obtained by ultra-high-performance liquid chromatography–mass spectrometry with electrospray ionisation (HPLC–ESI–MS). The treatment of Eimeria oocyst with OP extract and standard compounds (quercetin and oleuropein) leads to their lysis as shown by the release of substances absorbing at 273 nm. Results: Our results showed that the maximum number of reduced oocysts was recorded after 8 h of incubation of optimum OP extract, quercetin and oleuropein for different periods of time. Also, the number of Eimeria oocysts decreased considerably with increase concentrations after adding the optimum of OP extract in concentration ranging from 0.023 to 0.371 mg/ml. Positive correlation between the optimum OP extract concentrations and the number of Eimeria oocysts reduced was R2 = 0.959. From this in vitro experiment, it can be concluded that the OP extract possesses an anti-Eimeria spp activity. Conclusion: To our knowledge, this is the first time that quercetin and oleuropein were tested to evaluate their anticoccidial activity. The findings of this study showed that phenolic compound of OP extract tested separately possesses anti-Eimeria spp. effect. Further studies should be carried out to test its in vivo efficacy of the OP bioactive compounds in broiler chickens.

High-density polyethylene (HDPE) milk bottles are well-distinguished from other plastics in the mix-collected plastic waste and have potential to be closed-loop recycled. To evaluate this option, volatile substances present in various recycled HDPE (rHDPE) pellets and flakes from postconsumer milk bottles were analysed for similarities between different industrial recycling companies and batches. All substances found were classified in five different levels based on toxicity, from level I to level V (high toxicity). Chemicals present in the samples from different recyclers varied considerably, while those from different batches of a given recycler gave similar results. However, the study of rHDPE stream mixed with high volume of non-milk-bottles provided significant differences between batches. Washing the rHDPE twice and applying extra decontamination techniques reduced to a half the intensities for most chemicals detected, including two toxicity level V substances, butylated hydroxytoluene and diethyl phthalate. Nevertheless, other two high concern compounds, octocrylene, and 2-ethylhexyl-4-methoxycinnamate were not significantly reduced and thus deserve special attention when decontaminating rHDPE and evaluating its feasibility for food contact uses. Extra decontamination was able to reduce the intensities of 1-dodecene and 1-tetradecene. In total, 265 substances were detected in migration tests (95% ethanol and 3% acetic acid) and 58 of them were prioritized by toxicity. Regarding volatile migrants, rHDPE with low content of non-milk-bottle could be safe for direct contact with low-fat content food. For high-fat foods, the main concerns could come from 1-tetradecene, octocrylene, and 2-ethylhexyl-4-methoxycinnamate.