Search

Summary: The primary source of perfluoroalkyl substances (PFASs) exposure is the diet, mainly fish. Seabass (Dicentrarchus labrax) and seabream (Sparus aurata) are among the most consumed sea fish in Italy. Fish from Northern Italy lakes like perch (Perca fluviatilis) is of particular importance in terms of consumption volume, while Mediterranean shad (Alosa agone) and European whitefish (Coregonus lavaretus) represent niche consumption. These species too could be a cause of consumer exposure to PFAS. The study investigated the presence of PFASs in the above‐mentioned fish species through LC‐HRMS analysis. Only PFBA and PFOS were found both in lake and sea fish while PFBS was found only in lake fish. The found concentrations were used to estimate intake of PFOS, the only detected molecule of the four discussed in the last EFSA report. The Tolerable Weekly Intake of 4.4 ng kg−1 b.w. per week was never exceeded also for the 99th percentile consumers. [ABSTRACT FROM AUTHOR]

Continued use for industrial purposes of ever-new compounds compulsorily leads to the possibility of food contamination and risk for the consumer. Among the legacy and emerging contaminants, perfluoroalkyl substances (PFASs), used in the mid-20th century and still being implemented, are molecules of particular concern for their toxicity as endocrine disruptors, immunodepressants, possible carcinogens and liver and kidney toxicity. The main sources of PFAS exposure are water and food, particularly fish. In the European Union, European Food Safety Authority (EFSA) aimed the focus on 4 PFASs: perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA), perfluorohexane sulfonic acid (PFHxS) and perfluorooctane sulfonic acid (PFOS). In this study, canned tuna was the investigated matrix, as a highly consumed food. The study aimed to detect the presence of 18 PFASs in 75 paired batches of precooked tuna loins and canned tuna through ultra-high performance liquid chromatography-tandem high-resolution mass spectrometry (UHPLC-HRMS). Seven of the investigated PFASs were detected in the analyzed samples. Among them, just two of the four PFASs of which EFSA established a Tolerable Weekly Intake (TWI), i.e. PFOS and PFNA, were found in canned tuna. The risk characterization related to canned tuna resulted in an intake value much lower than the TWI for the average Italian consumer, but is a possible concern for high consumers, considering that canned tuna is not the only source of PFAS intake. [Display omitted] • A validated UHPLC-HRMS method for investigation of 18 PFASs was used. • A PFAS contamination comparison between pre-cooked loins and canned tuna was done. • PFOS, PFUnDA, and the sum of PFOS, PFOA, and PFNA concentrations were different. • Canned tuna displayed the highest levels of PFAS contamination. • Absence of cause of concern for average consumers of canned tuna was demonstrated. [ABSTRACT FROM AUTHOR]

BACKGROUND Fish consumption is increasing nowadays both because of its positive role for health due to the abundant presence of unsaturated fatty acids and for its use in many new food preparations (e.g. raw fillet used for uncooked sushi and sashimi dishes). The growing food industry and increased demand for the long‐term storage and preservation of food have created the need to develop methods that can easily track and preserve food freshness and safety throughout shelf‐life (production, storage, shipment, and consumption). While E‐nose technologies have already been used and tested for these purposes, scarce information is available in the literature on the feasibility of using other food devices to detect changes in perishable food like fish during shelf‐life in order to predict and correctly manage all food storage phases. The aim of the present study was to investigate the potential of Food Sniffer® portable devices to define the quality and safety of salmon fillet and burger (Salmo salar) packaged in modified atmosphere at two refrigerated conditions (4 and 8 °C). RESULTS: An increase in biogenic amines and volatile compounds especially ketones and alcohols were observed, with large amounts at final storage times of 8 °C temperature. CONCLUSION: The Food Sniffer® application was able to anticipate unacceptability conditions of salmon samples also correlated with chemical and microbiological parameters. This could represent a valid support for food industry and retail to manage perishable food commodities preventing possible food risk as well. © 2020 Society of Chemical Industry [ABSTRACT FROM AUTHOR]

Tuna is one of the most frequently consumed fish and, as a predator, can biomagnify pollutants. Metal and other elements pollution is an important worldwide concern. Based on these considerations, the aim of this work was to investigate the occurrence of As, Cd, Cr, Ni, Hg and Pb in tuna coming from different FAO areas to evaluate human exposure. The analysis was performed on muscle tissues through a quadrupole inductively coupled mass spectrometry. One hundred thirty-one samples were analysed. One red tuna from the Adriatic Sea and 11 yellow tunas exceeded Pb maximum levels (MLs) with a concentration ranging 0.31–0.86 mg kg−1; three red tunas from different Mediterranean sub-areas exceeded Hg MLs, with a concentration range 1.19 to 1.80 mg kg−1. All the Hazard Indexes (HIs) were lower than one, indicating that only a negligible health hazard could derive from the ingestion of tuna, for both average and high consumers. The risk of carcinogenicity from Cr is still under debate at the concentrations detectable in food. [ABSTRACT FROM AUTHOR]

Monitoring environmental contaminants in edible animal species is important for the assessment of environmental quality and for food safety as well. In this study, the occurrence of 2,3,7,8 dioxins, and furans, dioxin-like polychlorinated biphenyls, six non-dioxin-like polychlorinated biphenyl indicators (ndl-PCBs), seven polybrominated diphenylethers (PBDEs), four polycyclic aromatic hydrocarbons (PAHs) and four metals (As, Hg, Ni, Pb) was evaluated in 90 European eels (Anguilla anguilla) from Lake Garda. The results on eel samples showed a frequent contamination of dl-PCBs, found at concentrations higher than the maximum limit (ML) provided by European Union in 41 % of the eels. Two PBDE congeners (BDE 47 and BDE 99) were detected in almost all the samples. The contamination by PAHs was found negligible; only one sample had a high concentration of benzo[a]pyrene. Concerning metals, Pb showed concentrations higher than the maximum level (ML) in 77% of the samples, while Ni content could be a cause of acute toxicity due to dermatitis. Extreme consumers (95th percentile) are subjected to an actual risk attributable to dioxins, furans, and mainly dl-PCBs and PBDEs. The contamination of Lake Garda eels is therefore a matter of concern and a constant monitoring of the pollution levels of its freshwater is mandatory. [ABSTRACT FROM AUTHOR]

Glyphosate and glufosinate are broad spectrum herbicides, widely used in agriculture and in inhabited or industrialised areas, and aminomethylphosphonic acid is a degradation product of glyphosate. In 2015, the International Agency for Research on Cancer reported that glyphosate is a probable carcinogenic. In 2017, however, a scientific opinion of the European Chemicals Agency concluded that glyphosate is not proven to be carcinogenic, mutagenic or to have negative effects on reproduction. Nevertheless, aminomethylphosphonic acid was not considered. Due to their chemical-physical characteristics, these molecules present difficulties that have not yet allowed routine monitoring to be carried out. For these reasons, we developed and validated a simple and versatile liquid extraction, before IC-HRMS analysis, of three different complex matrices: honey, bass fish and bovine muscle. Among the satisfactory validation parameters, the LOQs in the range of 4.30–9.26 ng g−1 demonstrated high method sensitivity, compared to the few works present in literature. Finally, the method was applied to real commercial samples, which showed no traces of the selected pesticides. [ABSTRACT FROM AUTHOR]

Plastics are currently the most widely used and most suitable packaging material to meet quality and food safety, particularly for meat products, because of their perishable nature. Biopolymers are very interesting from the point of view of sustainability. This study focused on the application of biodegradable packaging (polylactic acid, PLA) for sliced salami in a protective atmosphere, as a potential replacement for the one currently used (polyethylene terephthalate, PET), monitoring the shelf life of the meat product through microbiological, chemical (colorimetric, pH and volatile compound determination) and sensory analysis. The results showed that the PLA-packaged salami maintained the red color throughout the entire shelf life; pH monitoring was essentially constant over time (from 5.63 to 5.70). Only one difference was detected at the end of shelf life regarding the main markers of product alteration (hexanal, 3-hydroxy-2-butanone, ethanol and 3-methyl-1-butanol), that were not sensory perceived remaining appreciated by the consumer panel. [ABSTRACT FROM AUTHOR]

Salmon consumption is increasing year by year. Salmon aquaculture is the fastest growing food production system in the world, and often uses feed mixed with antibiotics or other drugs. Feed can be also contaminated by environmental contaminants like persistent organic pollutants and organophosphorus pesticides that usually accumulate in fatty tissue, or emerging contaminants such as perfluoroalkyl substances (PFASs), that instead bioaccumulate in protein tissues. Therefore, there is the need to investigate the presence of antibiotics and environmental contaminants, with multi-class and multi-residue liquid chromatography-high resolution mass spectrometry and gas chromatography tandem mass spectrometry methods to monitor a broad spectrum of residues comparing between wild and farmed salmons. The presence of residues was encountered at a concentration range of 0.35-51.52 ng g−1 for antibiotics only in farmed salmon, 0.19-34.51 ng g−1 for PFASs and 0.26-9.01 ng g−1 for (polybrominated diphenyl ethers) PBDEs, and 0.19-5.91 ng g−1 for organochlorine pesticides with higher frequencies and concentrations in farmed fish. Finally, the risk deriving from salmon intake is low, being of minor concern only for PBDE 99 and perfluorooctanoic acid. [ABSTRACT FROM AUTHOR]

Parabens (PBs) are preservatives frequently used in cosmetics and personal care products as well as in the pharmaceutical and food industries due to their extensive defence mechanisms against multiple categories of microorganisms. Although they are considered safe when used within defined concentration limits, concern about their potential toxicity is still particularly active. Revealed as emerging pollutants, their incidence and behaviour in the aquatic environment have been studied, but there is only sporadic information when it comes to their extent and distribution in seafood. This study explores the presence of methyl- (MeP), ethyl-, propyl-, butyl-, and benzylparaben and their main degradation product 4-hydroxybenzoic acid (pHBA) in several fish species and bivalve samples with the aim to evaluate these food matrices as potentially important contamination sources of PB. Additionally, infant food containing fish was also enrolled in this survey: firstly, due to the absence of any information regarding this exceptionally important food item, and secondly, because of the necessity to estimate the PB content in the processed food. For this purpose, a fast, reliable and robust method was developed based on a simple liquid-liquid extraction followed by high-performance LC, coupled with a benchtop Q-Exactive Orbitrap high-resolution MS. The Q-Exactive parameters were carefully scheduled to achieve a balance between the optimal scan speed and selectivity, considering the limitations that are associated with generic sample preparation methodology. The method was validated through specificity, linearity, recovery, intra- and inter-day repeatability, LOD and LOQ. LOD and LOQ reached the ranges 0.65-3.5 and 2.15-11.7 ng g−1, respectively, while overall recovery ranged from 77% to 118%. The PBs were more frequently present in bivalves than in fish samples with MeP as the main PB detected. No PBs were found in infant food, but pHBA was observed in all samples. [ABSTRACT FROM AUTHOR]

Meat and meat products are included in a great number of human diets. However, the great consumption of meat needs to be controlled for the presence of traces of contaminants. The European Commission has not stated maximum limits for some environmental pollutants such as the perfluoroalkyl substances (PFASs) and polybrominated diphenyl ether (PBDE); the European Food Safety Authority (EFSA) Scientific Panel has recommended that more occurrence data for PFASs in food should be collected to improve the accuracy of future exposure calculations. Therefore, the distribution of PFASs and PBDEs trace contaminants from eight EU Member States were investigated through liquid chromatography coupled to high-resolution mass spectrometry (LC-HRMS) and Gas Chromatography-Mass Spectrometry (GC-MS/MS). No PFASs were detected, except perfluorooctanoic acid, in only one Austrian sample at the concentration of 0.531 ng g−1. PBDEs were detected in 3 out of 77 samples: one from Germany showed the presence of all congeners analysed in the concentration range 0.53-0.77 ng g−1, the others, from Netherland and Italy, respectively contained PBDE 153 (0.53 ng g−1) and PBDE 100 (0.62 ng g−1). The results show that the analysed samples do not pose a risk for human beings in regard to PFASs and PBDEs. Further studies are needed to keep monitoring their presence in foodstuff, as it has been suggested by European Commission. [ABSTRACT FROM AUTHOR]

Widespread antibiotic use and the antimicrobial resistance phenomenon demand new analytical methods and the use of non-conventional matrices increasingly necessary for safe food control. We present a method developed to detect six common antibiotics used in poultry breeding, in the unconventional matrix, feathers, compared to muscle and liver. The analysis for the presence of two β-lactams (penicillin V, amoxicillin), two fluoroquinolones (enrofloxacin, ciprofloxacin), one phenicol (thiamphenicol) and one macrolide (tylosin) was validated and achieved by HPLC–HRMS, with the ultimate aim to identify untargeted metabolites in broilers subjected to different therapeutic protocols. All the validated method parameters met the regulatory requirements. Muscle and liver were not effective matrices when the withdrawal periods were largely respected. Conversely, feathers proved a promising matrix for the detection of all the studied antibiotics, in the range of 8.72–1885.32 ng g −1 , except penicillin V. Like other nonconventional matrices, such as teeth, the antibiotics detected in feathers existed in their unmetabolised form. [ABSTRACT FROM AUTHOR]

Demand for honey is increasing, especially if it is organic and if its nutritional properties are linked to untreated environments in order to guarantee quality for health. Sources of contamination of honey can be divided into environmental and apicultural. Therefore, the distribution of persistent organic pollutants, pesticides and antibiotic residues from geographical areas with different contamination sources (high anthropic impact, intensive farming, husbandry and low anthropic impact) was investigated in order to confirm the potential transfer of xenobiotics into the supply chain and to give beekeepers tools for the selection of areas dedicated to organic production. The presence of polychlorinated biphenyls, polybrominated diphenyl ether and polycyclic aromatic hydrocarbons was confirmed, not only in proximity to highly urbanised centres, where the concentrations were higher, but in all environment contexts, confirming their ubiquity. No antibiotics or neonicotinoids were detected in 95 organic honeys, demonstrating the absence of apicultural treatments and consequently the good quality of honey of different areas. These results are important due to the undefined regulatory European situation on honey antibiotic limits. [ABSTRACT FROM AUTHOR]

Reviewing the presence of contaminant residues is important both for food safety and for monitoring of environmental pollution. Here, the occurrence of 6 polychlorinated biphenyls (PCBs), 15 organochlorine pesticides (OCPs), 7 polybrominated diphenyl ethers (PBDEs), 4 polycyclic aromatic hydrocarbons (PAHs) and 17 perfluoroalkyl substances (PFASs) was evaluated in mussels and clams. A liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) and an innovative QuEChERS extraction followed by gas chromatography-tandem mass spectrometry (GC-MS/MS) methods were developed, validated and applied. We demonstrate good linearity, repeatability and accuracy of these methods, confirming that they are suitable for the analyses of mollusc samples. The prevalence of PCBs, OCPs and PAHs was higher in mussels than in clams. For PFASs, contamination was higher in clams than in mussels. The samples were all compliant with the regulations, and, for the compounds without legislative limits, a risk assessment confirmed that the values were lower than the tolerable intakes. [ABSTRACT FROM AUTHOR]

Perfluoroalkyl substances (PFASs) contain one or more carbon-bound hydrogens substituted by fluorine. Since the 1950s, these compounds have been used to manufacture fat- and water-resistant fabrics, paper and food containers, and to produce photographic films, firefighting foams, detergents and insecticides. The widespread use and global distribution of PFASs, have led to their accumulation in the environment. Food, particularly fish and other seafood, is considered the main route of human exposure to PFASs. Consequently, the European Food Safety Authority (EFSA) recommends that more data be collected, to build a database on the contamination levels of the individual PFASs in food, to evaluate a reliable chronic risk to the European consumers. This requires high-sensitivity analytical methods, to increase the number of quantifiable samples and, thereby, improve the credibility of exposure assessments. In this context, the aim of the present research is to develop and validate a sensitive and specific method based on high-performance liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) analysis, to monitor the presence of 16 PFASs in Italian eels ( Anguilla anguilla ) from the Italian Lake Garda. The detection limits (CCα) and detection capability (CCβ) in the order of pg g −1 , the recoveries between 80 and 101% and the other validation parameters fulfilled the requirements of Commission Decision 657/2002/EC. The identification and quantification of PFASs, up to 11 in the same sample, showed a similar distribution among 90 eels. Perfluorooctane sulphonic acid (PFOS) and perfluorobutanoic acid (PFBA) were the analytes more frequently found in the eel samples (94 and 82%, respectively). [ABSTRACT FROM AUTHOR]

Filter feeders, like mussels and clams, are suitable bioindicators of environmental pollution. These shellfish, when destined for human consumption, undergo a depuration step that aims to nullify their pathogenic microorganism load and decrease chemical contamination. Nevertheless, the lack of contamination by drugs may not be guaranteed. Antimicrobials are a class of drugs of particular concern due to the increasing phenomenon of antibiotic resistance. Their use in breeding and aquaculture is a major cause of this. We developed a multiclass method for the HPLC–MS/MS analysis of 29 antimicrobials, validated according to the Commission Decision 2002/657/UE guidelines, and applied it to 50 mussel and 50 clam samples derived from various Food and Agricultural Organisation marine zones. The results obtained, indicate a negligible presence of antibiotics. Just one clam sample showed the presence of oxytetracycline at a concentration slightly higher than the European Union Maximum residue limit set for fish. [ABSTRACT FROM AUTHOR]

The antibiotic overuse in zoothechnics, due to prophylactic and therapeutic treatments, or to their growth-promoting activity, is a major cause for the onset of widespread antibiotic resistance. Of particular relevance to this study, is the antibiotic abuse in pig breeding. Despite the comprehensive literature on residue controls in pig muscle, data on pig urine, a non-invasive, on-farm collectable matrix, are lacking. Therefore, we validated an HPLC-MS/MS method to detect 29 antimicrobials from eight classes and applied it to 43 anonymous pig urine and muscle paired samples and fulfilled the parameters in agreement with the Commission Decision 2002/657/UE. The analytical limits were moreover much lower than the maximum residue limits (MRLs) required by the Commission Regulation 37/2010/UE. In the samples, antibiotics were usually detected at higher frequencies and concentrations in urine than muscle. Urine proved a useful tool to detect antibiotic administration and their excessive use in pig farming is depicted. [ABSTRACT FROM AUTHOR]

The worldwide loss of honeybee colonies may be due to their exposure to several contaminants (i.e., pesticides); such contamination may also have impacts on consumers’ health. Therefore, it is essential to develop quick and new methods to detect several pesticide residues in honey samples. In this study, the effectiveness of accelerated solvent extraction (ASE) was compared with QuEChERS methods for the analysis of 53 pesticides in organic honey by gas chromatography-triple quadrupole mass spectrometry. Two simple and rapid ASE methods with ‘in-line’ clean-up were optimised and then compared with QuEChERS. Hexane–ethyl acetate (Hex:EtAc) and Florisil were chosen as extraction solvent and retainer for the first ASE method respectively; acetonitrile and a primary–secondary amine phase (ACN-PSA) were selected for the second ASE method. The methods were validated according to the European Union SANTE/11945/2015 guidelines. The validation parameters showed that QuEChERS and ASE with PSA as retainer had better repeatability than ASE with Hex:EtAc and Florisil. In particular, QuEChERS and ASE (ACN-PSA) showed good recovery, according to the SANTE criteria, for the majority of investigated pesticides. Conversely, when ASE with Hex:EtAc and Florisil was used as the retainer, several compounds showed recoveries lower than the acceptable value of 70%. The ASE in-line method was finally applied to evaluate pesticide concentration in organic honey samples. [ABSTRACT FROM AUTHOR]

A method based on headspace solid-phase microextraction (HS-SPME) followed by GC-MS analysis was developed for the determination of underivatised acetic acid in fresh tuna fish muscle. Parameters such as the fibre selected and the extraction time and temperature were optimised and the linearity, detection limits and precision of the whole analytical procedure were assessed. The method was then applied to determine the acetic acid concentration in fresh yellowfin tuna muscles (Thunnus albacares) in order to evaluate the endogenous level and its variations during the shelf life under different storage conditions. A qualitative comparison was also made with variations in histamine levels to evaluate the possibility of the joint monitoring of acetic acid and histamine to identify fish stored in poor conditions. The caudal area always had a lower content of acetic acid than the ventral area, independent of the storage time and temperature. A difference was found between the 6- and 3-day time points and day 0 at a storage temperature of 8°C and between the 6-day time point and day 0 at a storage temperature of 0°C, independent of the anatomical area of the sampled tissue. The evaluation of acetic acid could represent an important approach in the field of food safety to detect the illicit use of acetic acid as an antibacterial preservative treatment or to eliminate the unpleasant smell of trimethylamine. [ABSTRACT FROM PUBLISHER]

Veterinary drugs usually have rapid clearance rates in the liver and kidney, hampering their detection in conventional matrices such as the liver or urine. Pharmacological principles such as esterification may be applied to facilitate the administration of veterinary drugs and increase drug half-life. Prednisolone, whose therapeutic administration is regulated for food producing animals in the EU, is available in its acetate form as well as nandrolone, a banned anabolic steroid, which may be obtained as nandrolone phenylpropionate and estradiol as a benzoyl ester. While the distribution and accumulation of lipophilic and hydrophilic substances in human teeth have been well documented, studies on residues in bovine teeth are lacking. We hypothesised that analysis of bovine teeth could be used to detect both regulated and banned veterinary drugs. Steroids may be illegally used as growth promoters in food producing animals, alone or combined with β2-agonists; therefore, we developed, and validated, in accordance with the Commission Decision 2002/657/EC, two analytical confirmatory LC-MS/MS methods to detect these classes of compounds following a unique liquid extraction procedure. Finally, we analysed teeth from three male Friesian veal calves treated with intramuscular estradiol benzoate, oral prednisolone acetate or intramuscular nandrolone phenylpropionate in combination with oral ractopamine, respectively, and from seven bovines from the food chain. Teeth from treated animals were positive for their respective drugs, with the exception of nandrolone phenylpropionate. One sample from a food chain bovine was positive for isoxsuprine, one of the seven β2-agonists studied. Non-esterified forms of the steroids were not found. These results demonstrate that bovine teeth are a suitable matrix for the determination of pseudoendogenous substances or illicit administration of veterinary drugs. [ABSTRACT FROM PUBLISHER]

The use of corticosteroids and anabolic steroids in food producing animals is regulated or banned in the European Union (EU). However, their use as growth promoters cannot be excluded. Milk replacers, considered by EU legislation as feeds, may be a good way of administration of these compounds. In order to improve the control of growth promoter utilization in animal husbandry and preventing possible consequences to animal welfare, we developed a method for multiresidue analysis of prednisolone, prednisone, dexamethasone, cortisone, cortisol, 17α- and 17β-boldenone and their precursor androstadienedione (ADD), testosterone, epitestosterone, 17α- and 17β-nandrolone, and trenbolone in powdered milk for calves. All analytes were extracted, after a common deproteinization and defatting sample pre-treatment, by a unique immunoaffinity column and analysed by liquid chromatography tandem mass spectrometry (LC–MS/MS) in both positive and negative electrospray ionization (ESI) modes. The method was validated according to the criteria of the Commission Decision 2002/657/CE. The analytical limits were from 0.39 to 0.73 ng mL −1 for the decision limit (CCα) and 0.46–0.99 ng mL −1 for detection capability (CCβ). The analysis of 50 samples of milk replacers for calves, always revealed the presence of cortisol and cortisone (average concentrations 2.56 and 1.06 ng mL −1 , respectively), frequently testosterone and epitestosterone (1.24 and 0.63 ng mL −1 , respectively), occasionally β-nandrolone (0.82 ng mL −1 ) and prednisolone (0.41 ng mL −1 ). The other anabolic steroids were never found. [ABSTRACT FROM AUTHOR]

A rapid, specific and simple procedure is proposed for the determination of free malonaldehyde (MA) contained in fish tissue. The method is the optimization of the reaction of MA with 2,3-diaminonaphthalene to afford a naphtodiazepinium ion that present a UV absorption at 311 nm, useful for MA determination by HPLC with UV detection. The reaction proceeds in the presence of 25% acetonitrile at 37 °C in 20 min at pH 2 using 2,4-pentanedione as internal standard. The method has been applied to homogenized samples of canned mackerel fillets that were treated with 2,3-diaminonaphthalene in an acidic aqueous:acetonitrile mixture. The produced naphtodiazepinium ion was extracted in acetonitrile by a salting-out homogeneous liquid–liquid extraction. A standard calibration was carried out in the range 0.625–10 nmol/g. The reliability of the procedure is demonstrated by linearity ( r 2 = 0.998), limit of detection (0.16 nmol/g), limit of quantification (0.22 nmol/g), repeatibility (RSD 5.57%), and intermediate precision (RSD 8.92%). [ABSTRACT FROM AUTHOR]

Nowadays food wrapping assures attractive presentation and simplifies self-service shopping. Polyvinylchloride (PVC)- and polyethylene (PE)-based cling-films are widely used worldwide for wrapping cheeses. For this purpose, films used in retail possess suitable technical properties such as clinginess and unrolling capacity, that are achieved by using specific plasticizers during their manufacturing process. In the present study, the main VOCs of three cling-films (either PVC-based or PE-based) for retail use were characterized by means of Solid-Phase Micro-Extraction and GC/MS. In addition, the effects of cling film type and contact time on the migration of VOCs from the films to four different PDO Italian cheeses during cold storage under light or dark were also investigated. Among the VOCs isolated from cling-films, PVC released 2-ethylhexanol and triacetin. These compounds can likely be considered as a "non-intentionally added substance". These same compounds were also detected in cheeses wrapped in PVC films with the highest concentration found after 20 days storage. The PE cling-film was shown to possess a simpler VOC profile, lacking some molecules peculiar to PVC films. The same conclusions can be drawn for cheeses wrapped in the PE cling-film. Other VOCs found in wrapped cheeses were likely to have been released either by direct transfer from the materials used for the manufacture of cling-films or from contamination of the films. Overall, HS-SPME is shown to be a rapid and solvent free technique to screen the VOCs profile of cling-films, and to detect VOCs migration from cling-films to cheese under real retail storage conditions. [ABSTRACT FROM AUTHOR]

• HPLC-Orbitrap lipidomics of irradiated meat was used for the food safety purposes. • Irradiation of chicken, turkey and mixed ground meat resulted in lipidome alterations. • Chicken, turkey and mixed ground meat were distinctly influenced by irradiation. • Characteristic oxidized phospholipids were identified in turkey irradiated meat. Meat irradiation is considered as an effective treatment that expose the advantageous effects on meat preservation. This research, based on untargeted LC-HR orbitrap MS-based lipidomics strategy was meant to estimate the alterations in lipid profile of irradiated chicken, turkey and mixed (chicken, turkey and pork) ground meat in order to evaluate if exists any food safety issue concerning the lipidome alteration. Special attention was paid on oxidation triggered by irradiation. All three matrices exhibited a characteristic lipidome profile which was affected differently by five levels of irradiation intensity. Overall, 345 lipids categorized into 14 subclasses were identified. Remarkably, the oxidized glycerophosphoethanolamines and oxidized glycerophosphoserines were identified in irradiated turkey meat, while for all three categories a characteristic diacylglycerols profile was recognised. Our analytical approach highlighted that the estimation of qualitative variations in lipid portion might be valuable in food inspection purposes, especially when the samples from animal origin are suspected on irradiation treatment. [ABSTRACT FROM AUTHOR]

A previously described derivatization method using trichlorophenylhydrazine was developed for the estimation of malonaldehyde measured by gas-chromatography (GC) with electron-capture detection. The precision and reliability of the procedure are improved here by the use of methylmalonaldehyde as internal standard and by the introduction of a diverter valve at the end of the capillary column to protect the electron-capture detector, respectively.The method was applied to determine malonaldehyde content in bovine plasma samples. [Copyright &y& Elsevier]

This study presents a comprehensive multimodal analytical study of an Egyptian ritual Bes-vase, of the 2nd century BCE employing cutting-edge proteomics, metabolomics, genetics techniques, and synchrotron radiation-based Fourier Transformed Infrared microSpectroscopy (SR µ-FTIR) to characterize organic residues of its content. We successfully identified the presence of various functional, bioactive, psychotropic, and medicinal substances, shedding light on the diverse components of a liquid concoction used for ritual practices in Ptolemaic Egypt. Using LC-MS/MS with a new methodological approach, we identified key proteins and metabolites, enabling the identification of botanical sources, confirmed by genetic sequences. Our analyses revealed traces of Peganum harmala, Nimphaea nouchali var. caerulea, and a plant of the Cleome genus, all of which are traditionally proven to have psychotropic and medicinal properties. Additionally, the identification of human fluids suggests their direct involvement in these rituals. Furthermore, metabolomics and SR µ-FTIR analyses also revealed the presence of fermented fruit-based liquid and other ingredients such as honey or royal jelly. The identification of specific chemical compounds, such as alkaloids and flavonoids, provides insight into the psychoactive and therapeutic uses of these in ancient ritual practices. This multidisciplinary study highlights the complexity of ancient cultures and their interactions with psychoactive, medicinal, and bioactive substances. These findings contribute to our understanding of ancient belief systems, cultural practices, and the utilization of natural resources, ultimately enhancing our knowledge of past societies and their connection to the natural world. [ABSTRACT FROM AUTHOR]

This study presents a comprehensive multimodal analytical study of an Egyptian ritual Bes-vase, of the 2nd century BCE employing cutting-edge proteomics, metabolomics, genetics techniques, and synchrotron radiation-based Fourier Transformed Infrared microSpectroscopy (SR µ-FTIR) to characterize organic residues of its content. We successfully identified the presence of various functional, bioactive, psychotropic, and medicinal substances, shedding light on the diverse components of a liquid concoction used for ritual practices in Ptolemaic Egypt. Using LC-MS/MS with a new methodological approach, we identified key proteins and metabolites, enabling the identification of botanical sources, confirmed by genetic sequences. Our analyses revealed traces of Peganum harmala, Nimphaea nouchali var. caerulea, and a plant of the Cleome genus, all of which are traditionally proven to have psychotropic and medicinal properties. Additionally, the identification of human fluids suggests their direct involvement in these rituals. Furthermore, metabolomics and SR µ-FTIR analyses also revealed the presence of fermented fruit-based liquid and other ingredients such as honey or royal jelly. The identification of specific chemical compounds, such as alkaloids and flavonoids, provides insight into the psychoactive and therapeutic uses of these in ancient ritual practices. This multidisciplinary study highlights the complexity of ancient cultures and their interactions with psychoactive, medicinal, and bioactive substances. These findings contribute to our understanding of ancient belief systems, cultural practices, and the utilization of natural resources, ultimately enhancing our knowledge of past societies and their connection to the natural world. [ABSTRACT FROM AUTHOR]

Antibiotics are widely used in livestock production as disease treatment, prevention and improve feeding efficiency. In this study three screenings and a multiclass method by Liquid Chromatography tandem Mass High Resolution Spectrometry (LC-HRMS) were developed and used to evaluate the antimicrobial substance incidence in 254 raw bovine milks involved in PDO cheese production in Northern Italy. The LC-HRMS results were compared to assess the frequency of false and negative results in term of reliability of screening methods. An investigation in relation to the quantified residues evaluating their possible negative impact on milk starter cultures in a simulated cheese-making process was presented. Lincomycin residues were observed in 30 samples, with 11.8% frequency and 17.29 ppb as mean value below its MRL. Three samples showed oxytetracycline respectively at 15.05, 0.82 and 1.59 ppb and two cefapirin and spyramycin at trace level. False positives with an acceptable frequency were observed by using the 3 kits confirming this approach useful for monitoring plans. Considering lincomycin, negative effect was demonstrated toward lactic acid bacteria activity in term of bacteria counts, pH and acidity during cheese making simulation. This represents a critical aspect considering both the economic value of PDO cheeses and the antibiotic resistance diffusion. • Antibiotic usage in animals may leave antibiotic residues in foodstuffs such as milk, egg and meat. • Screening test give great advantages in routine control. • Lincomycin was detected in several milk sample below its MRL. • Lincomycin led a negative impact on lactic acid bacteria. [ABSTRACT FROM AUTHOR]

Summary: The blue crab is one of the most invasive alien species in the Mediterranean Sea. Its remarkable surge in availability suggests an imminent increase in consumption. However, blue crabs are vulnerable to contamination by per‐ and polyfluoroalkyl substances (PFAS), known to accumulate in the food chain and pose health risks to humans. Data on PFAS contamination levels in blue crabs are a few. This study investigates 26 PFAS in 113 blue crabs by UHPLC‐HRMS. Results revealed higher concentrations in cephalothorax than in claws. PFHpA, PFHxS, PFOA, PFNA, PFOS, PFUnDA, PFDoDA, PFTrDA, PFHpS, and PFBA were among the most detected PFAS. Total PFAS mean concentration ranged from 0.65 to 2.61 ng g−1 ww. Three crabs exceeded maximum residue limits for PFOA, PFNA, and PFHxS. Statistical analyses suggested a correlation between contaminants presence and crab size. PCA highlighted the weight as a potential predictor of PFOS concentration. PFAS intake evaluation showed no risk for consumers. [ABSTRACT FROM AUTHOR]

Summary: Fish is well known for its perishable nature. Essential oils in food packaging seem to be safe and reliable both in terms of safety for the consumer and in terms of improving the shelf life of the product. This study aimed to evaluate the effects of two different essential oil vapours (one with rosemary and the other one with lemon extract) on three different types of fishery products (swordfish steaks, bluefin tuna steaks and Argentinian prawns) stored in a protective atmosphere packaging, monitoring the shelf life up to 8 days through microbiological, chemical and sensorial analyses. The results showed that the products preserved with the inclusion of essential oils have reached the end of the shelf‐life period respecting the process hygiene and food safety criteria, receiving a greater appreciation rating from the consumer panel at the end of shelf life for the prawns and swordfish samples with the addition of rosemary essential oils vapours, which instead highlighted the worst result at the end of shelf life for tuna. [ABSTRACT FROM AUTHOR]

The beneficial effects on human health of seafood are well known. However, seafood is a major source of exposition for consumers of most of the contaminants due to human activities such as breeding, industries, mining and agriculture: the overall level in biota, therefore seafood and particularly molluscs, dramatically increased over this last two centuries (Mozaffarian and Rimm, 2016). This study evaluates the presence of Cadmium, Lead, Mercury, Arsenic, Nickel and Chromium in mussels from the Italian mussel culture plants, and estimates the risk that Italian consumer undergoes eating these molluscs. A total of 30 mussel samples was collected at the wholesale fish market of Milan. The fishing area of origin were 37 FAO marine area (corresponding to Mediterranean Sea), particularly from FAO 37.2.1 Ligury, 37.2.2. North Adriatic, middle Adriatic, Puglia, 37.2.3 Lazio and Sardinia, and were collected from July 2016 to February 2017. (Fig.1). The analyses were done by using an Inductively Coupled Plasma Mass Spectrometer (ICP-MS), according to the Environmental Protection Agency (EPA) 3050B method. The concentrations (mg kg-1 wet weight) were shown as 25th, 50th (median), 75th and 100th (maximum concentration) percentiles. The sample concentrations were below the Maximum Levels (MLs) given by Commission Regulation (EC) No 1881/2006 (European Union, 2006) for Cadmium (0,15; 0,23; 0,08; 2,13 mg kg-1), Lead (0,14; 0,20; 0,32; 0,79mg kg-1) and Mercury (0,02; 0,03; 0,04; 0,16 mg kg-1), except one sample from south Adriatic sea, that showed Mercury concentration of 0.528 mg kg-1. Arsenic, Nickel and Chromium MLs are not stated by EU. Arsenic concentration was 4,00; 4,73; 5,58; 13,36 mg kg-1 and Nickel 0,27; 0,43; 0,69; 3,98 mg kg-1. Chromium was found only in 5 of 30 samples analysed with a concentration 0,00; 0,00; 0,00; 0,64 mg kg-1. Based on the tolerable intakes by EFSA (EFSA, 2014a, 2014b, 2015) and MLs by EU, Italian mussels do not pose a risk consumers. [ABSTRACT FROM AUTHOR]

Meat is a highly nutritious food but there is a lot of significant evidence of negative health outcomes related to its excessive consumption, especially for processed one. Among the variety of emerging contaminants of concern for human health, a key role is played by poly- and per-fluoroalkyl substances (PFASs), which show adverse effects in humans who are exposed to them through diet. In the present study, for the first time, 70 paired batches of pre-cooked and canned bovine meat were analysed by Liquid Chromatography coupled to High Resolution Mass Spectrometry to evaluate the presence and concentration of 18 PFASs. These data were used to assess Italian consumers' health risks by performing the PFAS intake evaluation. PFBA and PFOS were detected in the precooked and canned meat samples, with PFBA mean concentration of 0.22 ± 0.36 ng g−1, and

Volatile organic compounds (VOCs) have been proposed as one of the main factors for differentiating honeys from different botanical/floral origins. In this work, we investigated the volatile profile of honeys, commercially labeled as buckwheat honeys, from the Alps and its relationship with melissopalynological investigation. The results showed that buckwheat honey samples that contained, to different extents, buckwheat pollen grains on melissopalynological analyses showed similar VOCs profiles, distinguishing them from the other honey floral types analyzed. Among VO Cs identified, 3-methylbutanal, butanoic acid, pentanoic acid, and isovaleric acid were considerably greater in the buckwheat honey samples from the Alps. Other compounds were identified only in the honeys containing buckwheat pollen grains such as 3-methyl-2-buten-1-ol, 2-butanone, 2-hydroxy-3-pentanone, 4-methylpentanoic acid, 4-pentanoic acid, butanal, 2-methylbutanal, pentanal, dihydro-2-methyl-3(2H)-furanone, 5-methylfurfural, and cis-linalool oxide. These compounds give to buckwheat honey its characteristic aromatic and organoleptic properties and may be considered interesting as potential "variety markers" for botanical determination. [ABSTRACT FROM AUTHOR]

With the view of developing a gas-chromatographic (GC) determination of the 3-nitrotyrosine (NY)/tyrosine (Y) ratio as a marker of nitro-oxidative stress, different reagents were tested with the objective of obtaining a single volatile fluorinated product for each amino acid in a one-step derivatisation procedure. The heptafluorobutyric anhydride (HFBA)/heptafluorobutanol (HFBOH) mixture proved unsuccessful for the simultaneous analysis of NY and Y. The reaction with different chloroformates, isobutyl chlorofomate (iBuCF) and ethyl chloroformate (EtCF) in the presence of different perfluorinated alcohols, such as trifluoroethanol (TFEOH) and HFBOH, was investigated. A combination EtCF/fluorinated alcohols yielded derivatives of NY and Y as single peaks suitable for the GC determination of the NY/Y ratio. The different behaviours of the two amino acids in the employed reaction mixtures and the parameters influencing the results are discussed. [ABSTRACT FROM AUTHOR]

In view to develop a gas-chromatographic (GC) determination of the 3-nitrotyrosine (NY)/tyrosine (Y) ratio as a marker of nitro-oxidative stress, different reagents were tested with the objective of obtaining a single volatile fluorinated product for each amino acid by a one-step derivatization procedure. The heptafluorobutyric anhydride (HFBA) /heptafluorobutanol (HFBOH) mixture proved unsuccessful for NY and Y simultaneous analysis. The reaction with different chloroformates [isobutyl chlorofomate (iBuCF) and ethyl chloroformate (EtCF)] in the presence of different perfluorinated alcohols such as trifluoroethanol (TFEOH) and HFBOH was investigated. Combination EtCF/fluorinated alcohols yielded derivatives of NY and Y as single peaks suitable to the GC determination of the NY/Y ratio. The different behaviour of two amino acids in the used reaction mixtures and the parameters influencing the results were discussed. [ABSTRACT FROM AUTHOR]

Abstract: A method using headspace solid-phase microextraction (HS-SPME) combined with gas chromatography–mass spectrometry (GC/MS) was developed and validated for the extraction and quantification of hexanal content in butter (at ngg−1 level) during storage at 4°C. The variability of hexanal content among seasons of production and the influence of high extraction temperature on ex-novo formation of hexanal were also evaluated. The HS-SPME conditions were optimised and analytical parameters of the method (linearity, accuracy, and precision) demonstrate its usefulness. The reproducibility and accuracy of the quantitative analysis was assured by the use of D12-hexanal as internal standard. For the applications, the headspace was extracted using CAR/PDMS fiber for 180min at 4°C. Hexanal contents in samples during all storage period (shelf-life) and from butters produced in different seasons were analysed. Butter samples at the end of shelf-life and samples produced in August showed highest values of hexanal, confirming that the temperature both in storage and distribution phases represents a critical factor to maintain the quality of butter. [Copyright &y& Elsevier]

4-Hydroxy-2-nonenal (HNE) has been prepared from the corresponding dimethylacetal (HNE-DMA), in turn synthesized by a conventional approach with a few modifications of the experimental protocol and some improvements in the purification of the final product. In order to exploit the sensitivity of gas-chromatography with electron capture detector (GC-ECD) in the analysis of HNE derivatives, reaction of HNE with 2,4,6-trichlophenylhydrazine (TCPH) and 3,5-dichloro-phenylhydrazine (DCPH) was tested. Reaction with TCPH afforded a mixture of products, whereas with DCPH a single major product was formed that was prepared on a millimolar scale and purified. 1H-NMR analysis established that the derivative of HNE with DCPH is HNE 3,6-dichloro-phenylhydrazone, that can be used as standard for GC-ECD analysis [ABSTRACT FROM AUTHOR]

Large population studies estimated that the frequency of food allergies is increasing worldwide. In the last two decades, a 'second wave' of the allergy epidemic has emerged as a growing public health problem. EU regulation strengthened information to consumers about allergens in pre-packed food, since December 2014 it has been extended to non-prepacked foods by the Regulation (EU) No 1169/2011 of the European Commission. The present work aims to present a five-year survey on the presence of nine types of allergen in several foods, including food of animal origin and baby food. The concentration found for each irregular allergen is generally low, but some samples with no gluten indication contained a concentration above 10 mg kg−1 with the highest value of 138.5 mg kg−1 in a dietetic food, during the screening in 2017. These data underline the importance and the necessity of a complete food labelling to protect the majority of allergic individuals. [ABSTRACT FROM AUTHOR]

Dredging activities can lead to the re-suspension of contaminated sediments, resulting in a potential hazard for the whole ecosystem and also for human health. Six-month active biomonitoring was performed in order to monitor the trends of different classes of both legacy (organochlorine – OCPs – and organophosphate (OPs) compounds and polychlorinated biphenyls – PCBs) and emerging (polybromodiphenyl ethers – PBDE – and per- and polyfluoroalkyl substances – PFASs) organohalogen compounds, as well as polycyclic aromatic hydrocarbons (PAHs), in blue mussel (Mytilus edulis spp.) specimens transplanted at different depths in the Flekkefjord fjord. Such biomonitoring was performed to evaluate the efficacy of sediment restoration activities and to check for the potential environmental risk for the biota and food safety for human seafood. Negligible contamination by OCPs, OPs, PBDEs and PFASs was noted in mussels over the 6-month biomonitoring, while a notable increase in the concentrations of PCBs and PAHs occurred in mussels transplanted at 15 m depth in three sampling sites within the fjord, as a consequence of an undersea landslide which occurred during restoration activities. Levels of PCBs and PAHs suggested a potential risk for mussel predators and also for the human health, as they exceeded the limit set by the European Commission for the consumption of bivalve molluscs. These results confirm the reliability of active biomonitoring to flank dredging activities aimed at ecosystem restoration in order to monitor the trend of contaminants and to estimate the potential risk for the aquatic communities and human health. [ABSTRACT FROM AUTHOR]

Food safety becomes imperative when it aims to protect infants. The objective of this study was to investigate the presence of emerging contaminants of which some act as endocrine-disruptors in baby food. Persistent organic pollutants (POPs), perfluoroalkyl substances (PFASs), parabens and antibiotics were analysed in 112 baby food of different categories (meat, fish, vegetables, fruit, cheese). As regard POPs, PFASs and antibiotics, no residues were detected, while one sample showed methyl-paraben (4.14 ng g−1), whereas another three contained propyl-paraben (median 1.70 ng g−1). Special attention must be paid on parabens metabolites, as 4-hydroxybenzoic acid, the principal parabens metabolite, was detected in all samples (median 176.7 ng g−1). It may be present as a degradation product, but also, it can be released from vegetables and fruits during food processing. It is recommended to collect more data on natural vs non-natural occurrence of parabens and metabolites to evaluate the exposure of sensitive population vs ADI published by the European Food Safety Authority and European Medicines Agency. [ABSTRACT FROM AUTHOR]

The exposure to several compounds such as polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs), organophosphorus pesticides (OPs), polycyclic aromatic hydrocarbon (PAHs), perfluoroalkyl substances (PFASs) and polybrominated diphenyl ethers (PBDEs) is a public health issue. The European Union (EU) recommended that its member states monitor the presence of emerging contaminants, like PBDEs and PFASs, in food and in the environment to obtain an accurate estimation of exposure. The tissues of wild animals exposed to these compounds can represent a suitable indicator of environmental pollution. The aim of this work is to evaluate: (i) the occurrence of PCBs, PBDEs, PFASs, PAHs, OCPs and OPs in four game animals' meat (chamois, red deer, wild boar and roe deer); (ii) interspecies differences and (iii) human exposure. Muscle samples from seventy-nine animals were collected during the hunting season in a Northern Italy mountain area at altitudes ranging from 300 to 2500 meters above sea level. The analyses were performed with gas chromatography-mass spectrometry (GC-MS/MS) and ultra-performance liquid chromatography – tandem mass spectrometry (UHPLC-MS/MS). No PBDEs were found in the samples. OCPs, OPs and PCBs were detected in almost all samples at different concentration ranges, showing higher frequency in ungulate species than in wild boar. PFAs were found only in wild boar. Anthracene and benzopyrene, among PAHs, were found only in chamois, at low concentrations. The lack of an accurate pattern of exposure as well as variable consumption by hunters does not allow accurate risk characterisation. However, a low risk for consumers can be indicated due to the frequent detection of contaminants only at trace levels, the scarce prevalence of high concentrations of some contaminants and the low consumption of game animal meat. In conclusion, the organisation of a control plan on residues in game animals would be advisable. [ABSTRACT FROM AUTHOR]

Irradiation is a reputed efficient sterilizing method that demonstrated valuable effects on meat preservation. This research, based on qualitative untargeted HPLC-Orbitrap metabolomics approach, was intended to estimate the variations in global metabolome profile of irradiated chicken, turkey, and mixed (chicken, turkey, and pork) ground meat to assess the possible presence of a food safety issue concerning the metabolome alteration. Overall, 402 metabolites were identified, and all three matrices exhibited a specific metabolome profile that was not influenced remarkably by the application of five different levels of irradiation intensity. In particular, all three meat categories displayed the following common features: 1) free amino acids pool remained unaffected by irradiation 2) taurine appeared as the most important differentiator for all three category 3) amount of glutathione decreased 4) characteristic although minor, oxidative modifications of polyunsaturated free fatty acids occurred 5) intensified adenosine nucleotide degradation. The presented analytical approach highlighted the usefulness of meat metabolome profiling in distinction of irradiated meat from non-treated one. Metabolomics analysis did not diagnose any relevant negative impact of irradiation on meat safety issues, but contemporary has demonstrated alternations in few metabolic pathways. • HPLC-HRMS-Q-Orbitrap was used for metabolome profiling of irradiated meat. • Metabolomics is useful in distinguishing between irradiated and nonirradiated food. • The most important differentiators are involved in PUFA oxidation pathway. • Irradiation altered the AMP metabolism. • Metabolome profiling revealed no negative impact of irradiation on meat safety. [ABSTRACT FROM AUTHOR]

The Brazilian flora was widely used as source of food and natural remedies to treat various diseases. Bixa orellana L. (Bixaceae), also known as annatto, urucu, or achiote, is a symbol for the Amazonian tribes that traditionally use its seeds as coloured ink to paint their bodies for religious ceremonies. The aim of this study was to investigate the volatile organic compounds (VOCs) profile of B. orellana fresh fruits (in vivo sampled), dried seeds, wood, bark, and leaves analyzed with Headspace solid-phase microextraction coupled with gas chromatography and mass spectrometry. A screening on phenolic content (the Folin-Ciocalteu assay) and antiradical activity (DPPH assay) of seeds was also conducted. In addition, the repellent properties of seed extracts against Aedes aegypti L. were investigated. Volatile compounds detected in B. orellana samples consisted mainly of sesquiterpenes, monoterpenes, and arenes: α-humulene is the major volatile compound present in seed extracts followed by D-germacrene, γ-elemene, and caryophyllene. B. orellana proved to be a good source of antioxidants. Preliminary data on repellency against A. aegypti of three different dried seed extracts (hexane, ethanol, and ethanol/water) indicated a significant skin protection activity. A protection of 90% and 73% for hexane and ethanol/water extracts was recorded. [ABSTRACT FROM AUTHOR]

Abstract: An improved method for determination of 2-dodecylcylobutanone (DCB) in irradiated ground beef patties was developed. This method is based on a head-space solid-phase microextraction (HS-SPME) technique followed by gas-chromatography–mass-spectrometry (GC/MS) detection. SPME conditions were optimised: time and temperature for the adsorption of DCB on the polydimethylsiloxane (PDMS) fiber were set at 60min and 80°C, respectively. A matrix-matched standard calibration in the range 5–150ppb was carried out, using 2-pentylcyclopentanone as internal standard. Linearity (r 2 =0.9999), repeatability (8.4%), intermediate precision (13.6%), limit of detection (LOD) (1.5ppb), lower limit of quantification (LLOQ) (5ppb) demonstrated that the analytical procedure is fully reliable. The method was applied to irradiated samples in order to evaluate the dose–response effects. The concentration of DCB was quantified in beef patties irradiated at doses as low as 0.5kGy and was linearly increased up to 8kGy. [Copyright &y& Elsevier]

• HPIEC-SCD- high-resolution mass spectrometry (HRMS) for polyphosphates profiling. • HRMS proposed new linear/cyclic polyphosphates forms specific for food control. • HPIEC-SCD-HRMS platform revealed hexametapolyphosphate in some fishery products. Polyphosphates are permitted as food additives (Regulation EC No 1129/2011) but their undeclared utilisation is considered fraudulent. They improve water holding capacity of the seafood, preventing biochemical/physical changes during commercialization. The key objective of this study was the detection of polyphosphate in various seafood categories, by means of high-performance ion-exchange chromatography with suppressed conductometry (HPIEC-SCD) coupled to Q-Exactive Orbitrap high resolution mass spectrometry (HRMS-Orbitrap). Ten frozen cuttlefish samples did not reveal any treatment, while in ten frigate tunas, high concentration of orthophospate was found. Unambiguous hexametaphosphate presence was demonstrated in four prawn samples, while triphosphate was quantified (11.2 ± 4 ug/g) in another four prawn samples that contained orthophosphate (10225 ± 1102 ug/g), as well. Other samples sporadically encompassed polyphosphates profiles that varied according species and processing type. This analytical approach provided sustenance in better understanding regarding utilization of polyphosphates through HRMS fingerprinting of anionic species that would be specific in food safety control. [ABSTRACT FROM AUTHOR]

• 105 baby food of different typology were analysed for polar pesticides by IC-HRMS. • Glyphosate, glufosinate and their metabolites were not detected in baby food. • Sporadic presence of perchlorate was revealed, always under MRL. • Some fruit/vegetables preparation contained potentially problematic chlorate amount. • Chlorate content verified in some baby food exceeding the actual MRL. The incidence of endocrine disruptors, both possible (glyphosate and glufosinate), and demonstrated (perchlorate and chlorate), was estimated in baby food commodities (meat, fish, cheese, vegetable and fruit). Ion-chromatography coupled to high resolution mass spectrometry analysis of the 105 samples did not show traces of glyphosate, glufosinate or their metabolites, while in 10.5% of the samples a quantifiable amount of perchlorate was found. Some samples based on fruit and vegetables revealed a substantial amount of chlorate, especially the preparations that contained carrots and potatoes: five samples were in a concentration range of 40–120 μg kg−1, while one homogenized pear sample reached 372.2 μg kg−1. The pure meat samples revealed occasional chlorate appearance, with less than 10 μg kg−1. This is the first report of chlorate evaluated in various types of baby food and may serve as symptomatic data regarding its occurrence in infant/toddler diets. Therefore, effective monitoring programs and subsequent strict regulations are strongly required. [ABSTRACT FROM AUTHOR]

Simple Summary: In the world context of climate change and increasing food needs, it is of vital importance to preserve genetic resources in production ecosystems. On the Italian Alps that means conservation of local cattle breeds and maintaining of traditional alpine agro-pastoral practices. In particular, positive effects, such as preservation of fauna and flora biodiversity and greater appreciation by tourists, have been shown to correlate with mountain pastures. This study aimed to evaluate the relationships between different fatty acids in Original Brown cows' milk and cheese as well as the pattern of fatty acids that most contributes to discriminate between two different farming systems, in which the main difference was the practice, or not, of alpine summer-grazing. A multivariate statistical approach was used. Results indicated that the diet fed to animals, by influencing ruminal fermentation process and mammary gland de novo synthesis, is responsible for defining fatty acids characteristic profiles in dairy products. Findings also suggest that it is possible to build a reliable model based on specific fatty acids concentrations in order to identify pasture-raised or not dairy products. By this way, farmers who practice traditional agro-pastoral system could be easily recognized and adequately remunerated. This study aimed to evaluate the relationships between fatty acids and the pattern that most contributes to discriminate between two farming systems, in which the main difference was the practice, or not, of alpine summer-grazing. Milk and cheese were sampled every month in two farms of Original Brown cows identical under geographical location and management during no grazing season point of view in the 2018 season. Fatty acids concentrations were determined by gas chromatography. The principal component analysis extracted three components (PCs). Mammary gland de novo synthetized fatty acids (C14:0, C14:1 n9, and C16:0) and saturated and monosaturated C18 fatty acids (C18:0, C18:1 n9c) were inversely associated in the PC1; PC2 included polyunsaturated C18 fatty acids (C18:2 n6c, C18:3 n3) and C15:0 while conjugated linoleic acid (CLA n9c, n11t) and fatty acids containing 20 or more carbon atoms (C21:0, C20:5 n3) were associated in the PC3. The processes of rumen fermentation and de novo synthesis in mammary gland that are, in turn, influenced by diet, could explain the relationships between fatty acids within each PC. The discriminant analyses showed that the PC2 included the fatty acids profile that best discriminated between the two farming systems, followed by PC3 and, lastly, PC1. This model, if validated, could be an important tool to the dairy industry. [ABSTRACT FROM AUTHOR]