Strontium-90 (Sr-90) contamination in food is a major public health issue. Several radiochemical methods are available for the determination of Sr-90. However, the application of these procedures is not focused on solid foods, but only on liquid (milk, water, etc.) and environmental matrices, and they were not fully validated. The aims of this work were to establish and validate a fast, sensitive method for the determination of Sr-90 in solid food matrices such as meat and dairy products, seafood, vegetables, and animal feed, using a specific resin for extraction and ultra-low-level liquid scintillation counting for detection. The method was optimised and validated according to relevant legislation. Good analytical performance was obtained, including high specificity and linearity together with low measurement uncertainty (13.1%). The minimal detectable activity was 11 mBq kg −1 , and the mean repeatability (CV%) and recovery values were 10.7% and 100.1%, respectively. These parameters assured method applicability for official food safety controls. The method was applied to reference materials and submitted to proficiency test round to confirm its reliability for Sr-90 quantification in solid foodstuffs and feed. The newly established method may be broadly applicable to complex matrices.

The headspace-solid phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) technique was used to investigate 2-dodecylcyclobutanone (2-DCB) and 2-tetradecylcyclobutanone (2-TCB) as X-ray induced markers in irradiated dairy products. For the first time, an intensive study on several types of milk and cheeses, was carried out to evaluate both the suitability of this analytical technique for dairy products and how different factors related to these types of food, such as matrix composition, ripening time and technological processes, can affect 2-DCB and 2-TCB extraction. The results demonstrated that these analytes were identified in all types of irradiated samples, even if 2-TCB showed a lower sensibility than 2-DCB. Moreover, for both analytes, increasing irradiation dose over the experimental range of 0.5-5.0 kGy, a linear response was observed in all the matrices studied. The minimum dose level (MDL) and limit of detection (LOD), in irradiated and spiked samples, were 0.5 kGy and 5.0 mu g L-1, respectively. Furthermore, linear correlation between 2-DCB and 2-TCB contents was demonstrated. Finally, chemometric analysis highlighted the influence of ripening time and dairy technological processes on extraction capability of the two investigated analytes.

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. 137Cs was detected at a mean concentration of 0.53 Bq kg-1, and 40K, 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.

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).

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.

A sample of Roman glass found in Regio I, Insula 14, during the 1950's Pompeii excavation was examined by Raman and Fourier transformed infrared spectroscopy, scanning electron microscopy, and inductively coupled plasma mass spectrometry. The analyzed specimen was selected based on its intense blue color and its well-preserved aspect. The purpose of the work was the chemical characterization of Pompeii's glass in correlation to the actual knowledge of Roman glassmaking technology from the Mediterranean area. The results suggested that the Pompeii's glass was a soda-lime-silica glass, but with a higher calcium content that, given the low content of lead, was used to stabilize the glass. The sample was in origin produced most likely as non-decolorized primary raw materials from eastern Mediterranean sites. Moreover, the intense blue color was related to the use mainly of cobalt, present in a weighty amount, and likely used as important coloring agents in the ancient secondary glass-making workshop.

A Pompeian glass sample found in Reg. I, Insula 14 , during the 1950’s Pompeii excavation was examined by Raman and Fourier transformed infrared spectroscopy, scanning electron microscopy, and inductively coupled plasma mass spectrometry. The analyzed specimen was selected based on its intense blue color and its well-preserved aspect. The purpose of the work was the chemical characterization of Pompeii’s glass in correlation to the actual knowledge of Roman glassmaking technology from the Mediterranean area. The results suggested that the Pompeii’s glass was a soda-lime-silica glass, but with a higher calcium content that, given the low content of lead, was used to stabilize the glass. The sample was in origin produced most likely as non-decolorized primary raw materials from eastern Mediterranean sites. Moreover, the intense blue color was related to the use mainly of cobalt, present in a weighty amount, and likely used as important coloring agents in the ancient secondary glass-making workshop.

Diagnostic imaging has significantly grown over the last thirty years as indispensable support for diagnostic, prognostic, therapeutic and monitoring procedures of human diseases. This study explored the effects of low-dose X-ray medical diagnostics exposure on female fertility. To aim this, cumulus-oocyte complexes (COCs) recovered from the ovaries of juvenile sheep and human ovaries were used as complementary models for in vitro studies. In the sheep model, the effects of low-dose X-rays on oocyte viability and developmental competence were evaluated. In human ovaries originated from two age group (21–25 and 33–36 years old) subjects with gender dysphoria, X-rays effects on tissue morphology, follicular density and expression of apoptosis-related (NOXA, PUMA, Bcl2, Bak, γH2AX) and cell cycle-related genes (p21 and ki67) were investigated. It was noted that in sheep, the minimum dose of 10 mGy did not influence most of examined parameters at oocyte and embryo levels, whereas 50 and 100 mGy X-ray exposure reduced oocyte bioenergetic/oxidative activity but without any visible effects on oocyte and embryo development. In addition, blastocyst bioenergetic/oxidative status was reduced with all used doses. Overall data on human ovaries showed that low-dose X-rays, similarly as in sheep, did not alter any of examined parameters. However, in women belonging to the 33–36 year group, significantly reduced follicular density was observed after exposure to 50 and 100 mGy, and increased NOXA and Bax expression after exposure at 50 mGy. In conclusion, used low-doses of X-ray exposure, which resemble doses used in medical diagnostics, produce weak damaging effects on female fertility with increased susceptibility in advanced age.

Summary Due to food safety concerns, the European Food Safety Authority asked for novel approaches for identifying mechanically separated meat (MSM) in meat products. In this work, a novel and simplified approach for MSM identification in meat products is presented. This approach is based on the calcium and magnesium determination by suppressed cation‐exchange chromatography coupled to conductivity detection, after sample mineralisation. One hundred samples of meat products were analysed. The difference between calcium and magnesium concentration (MSM index ) was identified as the most significant parameter useful for discriminating the presence of MSM in the product. The approach was also validated by analysing simulated meat samples containing increasing percentages of MSM. Meat samples with MSM index higher than 390 mg kg −1 can be classified as MSM products, even if the MSM was obtained at high or low pressure. The protocol is applicable for MSM identification in meat products with MSM percentage higher than 25%.

T-2 and HT-2 toxins are secondary metabolites of various species of Fusarium. These molecules can have high potential toxic effects for human and animal health. In this work, ELISA and ultra performance liquid chromatography with fluorescence detection (UPLC/FLD) were implemented and validated as screening and confirmatory tests for the detection of these two toxins in cereal samples. The developed methods were tested by analyzing 100 samples of cereals by ELISA screening for reducing costs and analysis time and then using UPLC/FLD for confirmation purposes. Both methods met the performance criteria for sensitivity, linearity, selectivity, precision, and ruggedness, as reported in the European Decision No. 2002/657/EC and in Regulation (EC) No. 401/2006. The correlation between ELISA and UPLC/FLD approaches showed good results (r = 0.9056), confirming that these two techniques should be considered to be complementary in the official control activities of cereal and derived products.

N-nitrosamines (N-NAs), hazardous food contaminants, were submitted to an extensive electrochemical characterization of N-NAs in various mobile phases used as the supporting electrolyte and with metal and carbonaceous electrodes, in order to develop sensitive electrochemical detection methods to be applied in their post column analysis. N-NAs (N-nitrosodiethylamine, N-nitrosomorpholine, N-nitrosopyrrolidine, and N-nitro-sodiphenylamine) with both different structural characteristics and physico-chemical/reactivity properties were used as model compounds. Preliminary experiments by cyclic voltammetry at platinum (PtEs), gold (AuEs) and glassy carbon electrodes (GCEs) were performed to investigate their electrochemical behavior. The best performances were obtained either by AuEs in 20 mM methanesulfonic acid mobile phases (MSA) operating with pulsed amperometric detection (PAD) technique or by GCEs in organic mobile phases with direct current cathodic detection (DCCD) the latter proposed for the first time for the detection of N-NAs. The detection schemes were characterized in flow injection analysis (FIA) by the evaluation of some important performance parameters, such as limit of detection and response repeatability. For all the investigated N-NAs, PAD at AuEs in MSA and DCCD at GCEs in organic mobile phases showed detection limits in the range 0.8-1.2 mu M and 0.4-1.2 mu M respectively with RSDs of about 4%, showing the potential of the proposed electrochemical detection methods as an excellent alternative to the current N-NAs post column detection in liquid chromatography.

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.

This study aimed to verify the applicability of the EN 1787 method for the detection of irradiation in herbal ingredients used in Plant Food Supplements (PFSs). In matrices such as herbs and spices the main limit of the method is the presence of intrinsic radicals responsible for spurious signals leading to complex ESR spectra. To overcome this limit, before ESR measurement a treatment with alcohol has been proposed (Delincee and Soika, 2002; Ahn et al., 2012, 2014). As reported in the literature, this treatment is expected to reduce/eliminate the confounding signals so that the samples may be correctly classified. In this study the efficacy of the pre-treatment was tested on raw herbal ingredients largely used for PFSs, namely Camellia sinensis, Cinnamomum verum, Curcuma longa, Ginkgo biloba, Silybum marianum, Vaccinium myrtillus and Zingiber officinale. Non-irradiated and irradiated (5, 10 kGy) samples were analysed before and after pre-treatment. The results showed a general decrement of signal intensity. In some cases, this was associated with the elimination of some spurious signals, which, however, did not always ensue in an easier interpretation of the ESR spectra. Only for two matrices (Camellia sinensis and Vaccinium myrtillus) was alcoholic extraction crucial for the correct classification of the samples.

Debranning was applied to purple durum wheats to identify the debranning levels that provide potential functional flours naturally rich in bioactive compounds and low in toxic trace elements. Six debranning times were applied (30, 60, 90, 120, 150, 180 s) resulting in corresponding six debranned grains (DG-1 to DG-6). The content of total anthocyanins and polyphenols, and of ash, and essential (Cu, Mn, Zn, Se, Fe, Mo, Co) and toxic (Pb, Cd, Hg, As, Sn, Ni, Sr, V, Cr) trace elements and the antioxidant capacity were determined. In DG-1, 40% of the anthocyanins and 15% of the polyphenols were lost, and in DG-2 these losses were of 53% and 23%, respectively. At these DGs, the essential trace elements were mostly preserved (90.0% and 89.5%, respectively), while there was a decay of the toxic trace elements (11.0% and 24.5%, respectively). Debranning is confirmed as a useful technology to obtain improved flours.

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.

This paper reports the results of a study carried out to verify the applicability of the EN 1787 method, which uses the Electron Spin Resonance (ESR) technique for the identification of irradiated plant-origin foods with health benefits. The method was tested on samples of herbal ingredients of Plant Food Supplements (PFSs), nuts and fresh blueberries. Untreated and irradiated samples of Camellia sinensis (leaves) Ginkgo biloba (leaves), Glycine max (seeds), Silybum marianum (fruits), Vaccinium myrtillus (fruits), almonds, hazelnuts, peanuts, pistachios, walnuts and fresh blueberries were analysed. The work includes an inter-laboratory blind test involving five Italian laboratories that perform routine analyses for the official control of irradiated food. A total of 180 untreated and irradiated samples of PFS ingredients, nuts and fresh blueberries were analysed. The analyses on the irradiated samples were replicated even a long time after irradiation (up to two years depending on the matrix) to test the reliability of the method throughout the shelf life of the products. The results were matrix-dependent: all the 5 kGy irradiated nuts and the 1 kGy-irradiated blueberries were correctly classified, whereas herbal ingredients showed complex ESR spectra with spurious signals which often prevented the correct classification of the sample.

SummaryA rapid and simple procedure to detect irradiated food containing fat is proposed. This method is based on HS‐SPME coupled with GC‐MS to determine the presence of a radiolytic product in irradiated meats: 2‐dodecylcyclobutanone (2‐DCB) and is proposed as an alternative to EN 1785:2003, which is a long and complex procedure. The qualitative confirmation method is validated on different type of meats: chicken, turkey, duck, beef, pork on both nonirradiated and irradiated samples at different dose levels (0.05, 0.12, 0.5, 1.0 and 3.0 kGy) with a biological X‐ray irradiator. The validation parameters investigated are selectivity, minimum dose level (MDL), limit of detection (LOD), sensitivity and specificity. The MDL and LOD values were 0.5 kGy and 5.0 ng mL−1, respectively, for all matrices. No false positives or false negatives occurred, and 100% of samples were correctly identified. The results show that HS‐SPME GC‐MS is suitable for routine analysis.

Histamine contamination was evaluated on 474 batches (3130 determinations) of fish products collected in Puglia and Basilicata (southern part of Italy) during the years 2015–2019, using a high-throughput two-tier approach involving a screening (ELISA test) and confirmatory method (HPLC/FLD with o-phthalaldehyde derivatization). Histamine concentration >2.5 mg kg−1 was detected in 51% of total batches with the 2.5% of non-compliance. Except for two samples of fresh anchovies, all non-compliant samples were frozen, defrosted and canned tuna. Among 111 fresh tuna batches, 9 had a content of histamine between 393 and 5542 mg kg−1, and scombroid poisoning cases were observed after their consumption. Good quality canned tuna and ripened anchovies sold in Italy was observed. Furthermore, the analysis of the processing technology and storage practice critical points were reported in this study, with useful considerations to minimize the histamine risk for consumers. Finally, based on these results, several considerations about risk exposure were reported.