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A thresher shark poached by fishermen in the stretch of sea between the island of Ponza and the coast of Terracina (Lazio, Central Italy, Mediterranean Sea) and confiscated by the Italian health authorities was evaluated for the presence of chemical contaminants. Hg mean concentration of 2.1 mg kg -1 was found in muscle; speciation analysis confirmed it was almost in the toxic organic form of MeHg (2.0 mg kg -1 ). The Se:Hg molar ratio was <1 not protective against the toxic effect of Hg. 137 Cs was detected at a mean concentration of 0.53 Bq kg -1 , and 40 K, radioisotope of natural origin was found at 91 Bq kg -1 . Dioxins and PCBs were found in the common thresher shark at mean concentrations of 0.012 and 0.088 pg TEQ-WHO g -1 w.w. while NDL PCBs at 4.5 ng g -1 w.w., lower than limits set by European Regulation. The major concern is constituted by the presence of Hg twice the maximum limit set by EU Regulation, then the consumption of thresher shark flesh should be strongly discouraged., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

Durum wheat grains, which are mostly used for the production of pasta and several baked goods, represent a main source of vegetable proteins and calories. Concurrently, many contaminants, including toxic trace elements, may accumulate in them, posing a potential severe hazard to human health. In this context, for official control and food safety purposes, 346 samples of whole durum wheat imported into the Italian market from six countries (Australia, Canada, Kazakhstan, Russia, Turkey, and the United States) during the period 2015-2020 were analysed for cadmium (Cd), lead (Pb), and mercury (Hg) content using inductively coupled plasma mass spectrometry (ICP-MS). All the analysed samples were compliant with Food Agriculture Organization-World Health Organization and European Union regulations. The mean values were 0.0322 and 0.0162 mg kg -1 , respectively, for Cd and Pb, while all samples showed levels below the limit of detection (0.004 mg kg -1 ) for Hg. The results were construed in terms of seasonality, year, and country of production, and compared with reference tolerance values. Confirming previous exposure studies, the obtained data and the dietary intake assessment showed that durum wheat-based products may have a significant impact on exposure to Pb and Cd (20-50%) in the overall population, particularly in more sensitive and/or exposed subgroups (infants, toddlers, and females).

Sulfites are a class of chemical compounds, SO 2 releasers, widely used as additives in food industry, due to their antimicrobial, color stabilizing, antibrowning, and antioxidant properties. As the results of these pleiotropic functions they can be added to a broad range of products including dried fruits and vegetables, seafood, juices, alcoholic and nonalcoholic beverage, and in few meat products. Sulfites ingestion has been correlated with several adverse and toxic reactions, such as hypersensitivity, allergic diseases, vitamin deficiency, and may lead to dysbiotic events of gut and oral microbiota. In many countries, these additives are closely regulated and in meat products the legislation restricts their usage. Several studies have been conducted to investigate the sulfites contents in meat and meat products, and many of them have revealed that some meat preparations represent one of the main sources of SO 2 exposure, especially in adults and young people. This review discusses properties, technological functions, regulation, and health implications of sulfites in meat-based foods, and lays a special emphasis on the chemical mechanisms involved in their interactions with organic and inorganic meat components., (© 2020 Institute of Food Technologists®.)

Being an indirect approach, the standard method for the determination of polyphosphates (PPs) in food maybe characterized by high variability which can lead to significant errors in the final measurement. In this study, this method was validated and then compared to the ion chromatography-based approach. Method trueness and measurement uncertainty resulted comparable, while the precision of ion chromatography approach was higher. No "false positive" responses were obtained from ion chromatography analysis, while indirect photometry may cause "false positive" results (5% of analyzed samples). Regarding "false negative" results, this possibility maybe verified for all food types tested and for seafood when using indirect photometry and ion chromatography, respectively. The percentages of "false negative" samples were equal to 23.3% for indirect photometry and 10% for ion chromatography. In conclusion, the indirect photometry is a reliable method especially as "screening technique", while ion chromatography maybe used as a confirmatory technique, successfully., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

Due to food safety concerns, the European Food Safety Authority (EFSA) asked to identify useful parameters for identifying the mechanically separated meat (MSM). In this work, the 90 Sr levels of MSM products were assessed for evaluating the suitability of this parameter for MSM identification. Indeed, this contaminant may accumulate in animal bones and bone fragments may be present in MSM. One hundred samples of fresh meats and meat products composed of different MSM percentages and without MSM were analyzed by ultra-low-level liquid scintillation counting. The 90 Sr activity concentrations detected in meat products with high percentage of MSM were significantly higher ( p  ≥ 0.05) (0.099 Bq kg -1 ) than those of fresh meats (0.024 Bq kg -1 ) and meat products containing low percentage of MSM (0.011 Bq kg -1 ). The percentage of correct MSM identification was 61%. In order to increase this percentage and to develop a new tool of investigation, the 90 Sr was elaborated in combination with other three parameters: 88 Sr, Ca and ash percentage, through a multivariate approach. The precision of this tool of investigation was significantly increased (87%), higher than the reference method (Ca level) (76%), representing a valid novel approach in the identification of MSM products., Competing Interests: Conflict of interestThe authors declare that they have no conflict of interest., (© Association of Food Scientists & Technologists (India) 2019.)

Di-(2-ethylhexyl) phthalate (DEHP) is a commonly used plasticizer with endocrine-disrupting properties. In this study, we used an equine model to investigate DEHP concentrations in ovarian follicular fluid (FF), and to determine the effects of exposure of oocytes to potentially toxic concentrations of DEHP during in vitro maturation (IVM) on embryo development and quality. Embryo development was evaluated using time-lapse monitoring (TLM), a photomicroscopic tool that reveals abnormalities in cleavage kinetics unobservable by conventional morphology assessment. Blastocyst bioenergetic/oxidative status was assessed by confocal analysis. The possibility that verbascoside (VB), a bioactive polyphenol with antioxidant activity, could counteract DEHP-induced oocyte oxidative damage, was investigated. DEHP was detected in FF and in IVM media at concentrations up to 60 nM. Culture of oocytes in the presence of 500 nM DEHP delayed second polar body extrusion, reduced duration of the second cell cycle, and increased the percentage of embryos showing abrupt multiple cleavage, compared with controls. Mitochondrial activity and intracellular levels of reactive oxygen species were reduced in blastocysts from DEHP-exposed oocytes. VB addition during IVM limited DEHP-induced blastocyst damage. In conclusion, DEHP is detectable in equine FF and culture medium, and oocyte exposure to increased concentrations of DEHP during IVM affects preimplantation embryo development. Moreover, TLM, reported for the first time in the horse in this study, is an efficient tool for identifying altered morphokinetic parameters and cleavage abnormalities associated with exposure to toxic compounds., (© 2019 Wiley-Liss, Inc., A Wiley Company.)

The use of food dyes in meat is subject to regulations, due to food safety concerns. A reliable method for the determination of 12 food dyes (Amaranth, Ponceau 4R, Carmine, Ponceau SX, Ponceau 3R, Allura Red AC, Carmoisine, Erythrosine, Sudan I, Sudan II, Sudan III and Sudan IV) in meat products using high performance liquid chromatography coupled to UV-diode array detection was developed, optimized and fully validated. The extraction was accomplished using acetonitrile, methanol, water, ammonia, 50:40:9:1 (v/v/v/v) as the solvent, and an ultrasonic bath. Chromatographic separation was achieved using a C 18 RP column and samples eluted with a gradient acetate-acetonitrile mobile phase. Good analytical performance was obtained, in terms of selectivity, sensitivity, accuracy and ruggedness. Both method precision (CV% range: 6.2%-18.0%) and recovery (range: 86.4%-105.0%) complied with Decision 657/2002/EC, suggesting the procedure could be applied successfully for analyses of meat products in the European Union., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

The use of food dyes in meat is regulated by the current European and non-European legislation, due to several food safety concerns. A reliable method for the quali-quantitative determination of 12 food dyes (Amaranth, Ponceau 4R, Carmine, Ponceau SX, Ponceau 3R, Allura Red AC, Carmoisine, Erythrosine, Sudan I, Sudan II, Sudan III and Sudan IV) in meat products, by high performance liquid chromatography coupled to UV diode array detection is presented. The extraction was accomplished by using acetonitrile, methanol, water, and ammonia, 50:40:9:1 (v/v/v/v) as the solvent and ultrasonic bath. The chromatographic separation was obtained with a C 18 RP column eluted by a gradient of acetate buffer/acetonitrile. Good analytical performances characterized this method (Table 1), in terms of selectivity, sensitivity, accuracy and ruggedness. Both method precision (CV% range: 6%-15%) and recovery percentages (range: 86%-105%) resulted in compliance with Decision 2002/657/EC, and the expanded measurement uncertainties, estimated by a bottom-up approach, were in the range 6%-20%. All these results demonstrated that the procedure can be applied successfully for confirmation analyses of commercial meat products. •12 food dyes were determined in meat by new HPLC/UV-DAD method.•The analytical method was fully validated for accurate confirmation analyses.•Method accuracy, sensitivity, selectivity and ruggedness resulted satisfactory.

Strontium-90 (90Sr) is a fission product, resulting from the use of uranium and plutonium in nuclear reactors and weapons. Consequently, it may be found in the environment as a consequence of nuclear fallouts, nuclear weapon testing, and not correct waste management. When present in the environment, strontium-90 may be taken into animal body by drinking water, eating food, or breathing air. The primary health effects are bone tumors and tumors of the blood-cell forming organs, due to beta particles emitted by both 90Sr and yttrium-90 (90Y). Moreover, another health concern is represented by inhibition of calcification and bone deformities in animals. Actually, radiometric methods for the determination of 90Sr in animal bones are lacking. This article describers a radiochemical method for the determination of 90Sr in animal bones, by ultra low-level liquid scintillation counting. The method precision and trueness have been demonstrated through validation tests (CV% = 12.4%; mean recovery = 98.4%). Detection limit and decision threshold corresponding to 8 and 3 mBecquerel (Bq) kg-1, respectively, represent another strong point of this analytical procedure. This new radiochemical method permits the selective extraction of 90Sr, without interferences, and it is suitable for radiocontamination surveillance programs, and it is also an improvement with respect to food safety controls.

The profile of 18 trace elements was traced in 68 milk samples collected from buffalo farms in the territory known as the "Land of Fires" in the Campania region (Italy). This area has been polluted by the illegal dumping in fields of industrial or domestic waste, wich is sometimes then burned spreading toxic contaminants. Milk from buffaloes raised on rural farms might be a good indicator of environmental contamination risk in the human food chain. Trace element analysis in milk was performed using mass spectrometry. One milk sample was found to be non-compliant due to high Pb concentration. In the absence of threshold values for the elements, established through legislation, the results were compared with similar studies from other countries, and in most cases the content determined in this study was in agreement with values reported elsewhere and do not represent a risk to human health., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

Cadmium is a highly toxic heavy metal with negative effects on oocyte fertilization. The aim of this study was to analyse whether cadmium-induced impairment of fertilization is caused by mitochondria dysfunction and oxidative stress in the cumulus-oocyte complex (COC). Preliminarily, 19 trace element levels were measured in ovaries from juvenile and adult ewes and age-related cadmium ovarian bioaccumulation at nanomolar concentrations was found. COCs from juvenile and adult ewes, exposed during in vitro maturation to 1nM or 100nM CdCl 2 , and subjected to in vitro fertilization showed significantly lower fertilization rates in exposed COCs compared with controls. In vitro matured exposed and control COCs underwent confocal microscopy analysis of mitochondria activity and reactive oxygen species (ROS) levels and lipid peroxidation (LPO) assay at cumulus cell and oocyte level. In both age groups, cadmium at nanomolar concentrations induced cumulus-oocyte mitochondria over-activity and oxidative damage which were related to impaired oocyte fertilization., (Copyright © 2017 Elsevier Inc. All rights reserved.)

Concentration values of 24 elements (Al, As, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe, Ge, Hg, Mn, Mo, Pb, Sb, Se, Sn, Sr, Ti, Tl, U, V, and Zn) were determined in 72 honey samples produced in Italy by inductively coupled plasma mass spectrometry (ICP-MS). Considering the recommended established heavy metal daily intakes for humans, in this perspective, an equilibrated and ordinary honey consumption should not be considered matter of concerns for human health, even if particular attention should be addressed if honey is consumed by children, due to different maximum daily heavy metal intakes. Chemometric analysis of the results obtained highlights heavy metal content differences in honey samples obtained from notoriously polluted zones, confirming then that honey can be considered a bio-indicator of environmental pollution. Finally, Pearson coefficients highlighted correlations among element contents in honey samples.

(90)Sr is considered an important contaminant relating to food supply chains. In this study, 176 liquid and 260 solid foods, were analysed in order to quantify (90)Sr. Through ruggedness tests, the application field of radiochemical methods used was extended successfully to all most important types of foodstuffs. Regarding liquid matrices, milk samples resulted the most important indicator about (90)Sr contamination, with mean (90)Sr activity concentration equal to 0.058BqL(-1). Among other liquid foods, wine/spirits and livestock watering resulted the most contaminated, with mean contamination levels equal to 0.022 and 0.035BqL(-1), respectively. Concerning solid matrices, cheeses produced from sheep's milk and animal feeds resulted the most contaminated (mean levels: 1.237 and 1.557Bqkg(-1), respectively). Meat products and seafood showed contamination levels not significant within this survey; while, among vegetables, cacao/chocolate and spices resulted in contamination levels comparable with those of cheese obtained from milk of cows origin., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

In this work, environmental heavy metal contamination in the Val d'Agri area of Southern Italy was monitored, measuring the accumulation of 18 heavy metals (U, Hg, Pb, Cd, As, Sr, Sn, V, Ni, Cr, Mo, Co, Cu, Zn, Ca, Mn, Fe, and Al) in the organs of animals raised in the surrounding area (kidney, lung, and liver of bovine and ovine species). Val d'Agri features various oil processing centers which are potentially a significant source of environmental pollution, making it essential to perform studies that will outline the state of the art on which any recovery plans and interventions may be developed. The analysis was carried out using official and accredited analytical methods based on inductively coupled plasma mass spectrometry, and the measurements were statistically processed in order to give a contribution to risk assessment. Even though five samples showed Pb and Cd concentrations above the limits defined in the European Commission Regulation (EC) No 1881/2006, the mean concentrations of most elements suggest that contamination in this area is low. Consequently, these results also suggest that there is no particular risk for human exposure to toxic trace elements. Nevertheless, the findings of this work confirm that element accumulation in ovine species is correlated with geographical livestock area. Therefore, ovine-specific organs might be used as bioindicators for monitoring contamination by specific toxic elements in exposed areas.

Element profiling is an interesting approach for understanding neurodegenerative processes, considering that compelling evidences show that element toxicity might play a crucial role in the onset and progression of Alzheimer's disease (AD). Aim of this study was to profile 22 serum elements in subjects with or at risk of AD. Thirtyfour patients with probable AD, 20 with mild cognitive impairment (MCI), 24 with subjective memory complaint (SMC) and 40 healthy subjects (HS) were included in the study. Manganese, iron, copper, zinc, selenium, thallium, antimony, mercury, vanadium and molybdenum changed significantly among the 4 groups. Several essential elements, such as manganese, selenium, zinc and iron tended to increase in SMC and then progressively to decrease in MCI and AD. Toxic elements show a variable behavior, since some elements tended to increase, while others tended to decrease in AD. A multivariate model, built using a panel of six essential elements (manganese, iron, copper, zinc, selenium and calcium) and their ratios, discriminated AD patients from HS with over 90% accuracy. These findings suggest that essential and toxic elements contribute to generate a distinctive signature during the progression of AD, and their monitoring in elderly might help to detect preclinical stages of AD.

Here, we propose a novel strategy that combines a typical ultra high performance liquid chromatography (UHPLC), data-independent mass spectrometry (MS(E)) workflow with traveling wave ion mobility (TWIM) and UV detection, to improve the characterization of carotenoids and chlorophylls in complex biological matrices. UV detection selectively highlighted pigments absorbing at specific wavelengths, while TWIM coupled to MS was used to maximize the peak capacity. We applied this approach for the analysis of pigments in different microalgae samples, including Chlorella vulgaris, Dunaliella salina, and Phaeodactylum tricornutum. Using UHPLC-UV-MS(E) information (retention time, absorbance at 450 nm, and accurate masses of precursors and product ions), we tentatively identified 26 different pigments (carotenes, chlorophylls, and xanthophylls). By adding TWIM information (collision cross sections), we further resolved 5 isobaric pigments, not resolved by UHPLC-UV-MS(E) alone. The characterization of the molecular phenotypes allowed us to differentiate the microalgae species. Our results demonstrate that a combination of TWIM and UV detection with traditional analytical approaches increases the selectivity and specificity of analysis, providing a new tool to characterize pigments in biological samples. We anticipate that such an analytical approach will be extended to other lipidomics and metabolomics applications.

90 Sr is considered as a dangerous contaminant of agri-food supply chains due to its chemical affinity with Calcium, which makes its absorption in bones easy. 90 Sr accumulation in raw materials and then in final products is particularly significant in relationship to its ability to transfer into animal source products. The radionuclides transfer ( 137 Cs and 90 Sr) from environment to forages and then to products of animal origin (milk, cow and pork meats) was studied and evaluated in different studies, which were carried out in contaminated areas, from Chernobyl disaster until today. In the present work, the development and validation of a radiochemical method for the detection of 90 Sr in different types of animal feed, and the application of this technique for routinely control activities, are presented. Liquid scintillation counting was the employed analytical technique, since it is able to determine very low activity concentrations of 90 Sr (<0.01 Bq Kg -1 ). All samples analysed showed a 90 Sr contamination much higher than method detection limit (0.008 Bq kg -1 ). In particular, the highest mean activity concentration was registered in hay samples (2.93 Bq kg -1 ), followed by silage samples (2.07 Bq kg -1 ) and animal feeds (0.77 Bq kg -1 ). In fact, all samples were characterized by 90 Sr activity concentrations much lower than reference limits. This notwithstanding, the necessity to monitor these levels was confirmed, especially considering that 90 Sr is a possible carcinogen for human.

Lead, cadmium and mercury are non-essential heavy metals that may interfere with biological systems, exhibiting high toxicity to human and marine biota. Due to bioaccumulation of heavy metals in the food chain, seafood may concentrate high levels of these contaminants since they are often at the top of aquatic food chain. In this study, 342 seafood samples, subdivided into four categories (bivalve molluscs, cephalopod molluscs, blue-fish and other sea fish), were analysed by inductively coupled plasma mass spectrometry, in order to assess the levels of lead, cadmium and mercury. Contamination levels higher than allowable limits were verified. In particular, two bivalve mollusc samples were non-compliant for lead and cadmium, four cephalopod mollusc samples non-compliant for cadmium and 14 samples (4 blue-fish and 10 other sea fish) non-compliant for mercury. This survey confirmed the necessity to perform routinely controls related to this type of food inspection.

Strontium-90 is a hazardous radionuclide derived from nuclear fission processes, and it decays emitting high-energy beta-particles forming yttrium-90. It may be easily absorbed in humans through several food supply chains, since it is chemically similar to some important biological elements such as potassium and calcium. In this work an analytical method for the determination of radiostrontium in milk by liquid scintillation counting was developed in order to obtain a precise quantification at low activity concentration levels. Moreover, a full validative approach was applied to confirm method reliability. Good analytical performance was obtained by developing an in-house validation model according to Regulation 882/2004/EC and Decision 657/2002/EC with a good selectivity, a decision threshold and detection limit corresponding to 0.003 and 0.006 Bq l⁻¹ (α = β = 0.05) respectively, a repeatability value, expressed as CV%, equal to 13%, a mean recovery value equal to 102.5% and a measurement uncertainty equal to 11.5%. Strontium and yttrium chemical yields were determined by a reliable analytical method by inductively coupled mass spectrometry, assuring a suitable correction of final result. The results of the method validation, combined with a quality control assurance, performed on a reference material, demonstrated that the procedure represents a substantial improvement in the determination of ⁹⁰Sr relating to accurate confirmation analyses.

This study shows an exhaustive comparison of different methods, based on luminescence techniques, to identify X-ray irradiated oysters at five different dose levels in the range 0.1-2 kGy and suggests a simple, fast and sequential routine analysis protocol. A total number of 50 oysters from North Sea, including 10 control samples, were analysed by using two photo-stimulated luminescence (PSL) methods (named A and B) and three thermoluminescence (TL) methods (named C, D and E), either on constituents or contaminating minerals from shells and intestines. Setting a lower threshold value T1 (1000 counts/60s) all of control specimens gave negative screening results while photo counts from irradiated samples were found to be higher than upper threshold T2 (4000 counts/60s), except at the lowest dose level 0.1 kGy for procedure A. All PSL calibrated analysis were successful and a sensitivity index was also determined to better classify obtained data according to the revised European Standard (EN 13751:2009). TL ratios, Glow 1 over second Glow 2, the latter after irradiating at 1 kGy and remeasuring the same minerals for each sample, showed values less than 0.1 related to untreated samples or higher than 0.1 for irradiated ones. Reported procedures were also tested over 60 days, longer than oyster shelf life confirming the applicability and feasibility of the proposed methods., (Copyright © 2012 Elsevier Ltd. All rights reserved.)

Food irradiation is a preservation method that has been approved by the European Union for a limited number of foods or food products and within a limited range of doses. European Community legislation states that all foods or food ingredients treated in this manner and authorized for sale in the European Union must be clearly labeled, and that market-level inspections must be carried out to ensure compliance with this regulation. To improve detection of irradiated foods, we evaluated the efficacy of electron spin resonance (ESR) spectroscopy for the identification of seafood that had been subjected to irradiation. Three fish species were tested: gilthead sea bream, cod, and swordfish. For each species, 18 samples of flesh-containing bone were analyzed after either irradiation at 0.5, 1, or 3 kGy or no irradiation (control). Induced radicals in irradiated samples produced distinct ESR signals that allowed differentiation from non-irradiated samples. Within the dose range tested, a linear dose-response relationship was observed (R(2) > 0.94). The gilthead sea bream displayed the highest radiosensitivity. The analytical procedure was validated and successfully used for the routine monitoring of locally marketed seafood. The main aims of the study were to develop a reliable tool for the enforcement of the proper labeling of irradiated foods and to obtain preliminary data on compliance with current laws in the Italian market.