Search

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 aim of this work was to verify the applicability of the European Standard EN 13751, based on Photo-Stimulated Luminescence (PSL) and the European Standard EN 1788, based on Thermoluminescence (TL), for the detection of irradiation in plant food supplement (PFS) ingredients, nuts and fresh fruits with health benefits. In particular, in this work, herbal ingredients (Camellia sinensis, Ginkgo biloba, Glycine max, Silybum marianum, Vaccinium myrtillus), almonds, hazelnuts, peanuts, pistachios, walnuts and fresh blueberries, papaya and mango, were analyzed by both stimulated luminescence methods. To verify the reliability of the methods in detecting the treatment over time, the analyses were replicated after irradiation within the product shelf life. The PSL screening method allowed to correctly identify blueberries, nuts and raw materials of PFS but failed with dried herbal extracts, mango and papaya, due to their low content of silicates. To validate the procedure elaborated during the preliminary study, blind tests, involving several national laboratories of the official control, were organized. The tests confirmed the limits in detecting dried extracts, mango and papaya by PSL technique. TL method resulted suitable as a confirmatory method for all the matrices of the study.

A 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.

Food irradiation is used to preserve food from pathogenic microorganisms, deterioration and to extend shelf life. The EU legislation states that any irradiated food or food ingredients must be labeled with the word “irradiated”. The ESR spectroscopy is a powerful tool to enhance official checks; hence, it has been used to detect irradiated hazelnuts. The results from the ESR studies on hazelnuts before and after X-ray irradiation are reported. Before irradiation hazelnuts exhibit one singlet ESR line characterized with a g-factor of 2.0046 ± 0.0006. After irradiation, a typical “cellulose-like” triplet ESR spectrum appears. To investigate the radio-induced free radical stability, the peak-to-peak amplitude of the ESR satellite signals was considered. Fading measurements indicate that the intensity of the ESR spectra of hazelnuts is reduced to about 70% after 30 days. In addition, the microwave power behavior and a dose–response relation were investigated. The study confirmed the applicability of ESR technique to detect irradiated hazelnuts also when a long time after treatment was passed.

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.

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.

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&ndash, 2019, using a high-throughput two-tier approach involving a screening (ELISA test) and confirmatory method (HPLC/FLD with o-phthalaldehyde derivatization). Histamine concentration &gt, 2.5 mg kg&minus, 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&minus, 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.

Sulfites are a class of chemical compounds, SO2 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 SO2 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.

Previous studies have demonstrated that mushrooms, due to their ability to absorb environmental elements and to grow in almost every habitat, can be heavily contaminated by radioactive isotopes, especially when radiological emergencies like the Chernobyl accident occurs. In this work two species of edible mushrooms have been considered -Boletus edulis and Amanita caesarea-imported in Italy from two different Balkan areas: Macedonia and Albania/Kosovo. The different behavior of the two species in accumulating radiocesium has been investigated, showing that the first variety of mushrooms is more contaminated with Cesium-137 than the second. It has been verified that there were no observed differences in radiocontamination levels between mushrooms originating from different areas. During the period 2008–2017, the mean Cesium-137 activity in edible mushrooms has followed a decreasing trend, whose rate is faster than the natural one. Two different consumption scenarios were considered: in both cases the consumption of mushrooms proved to be non-dangerous for humans.

Samples of non-irradiated walnuts exhibit a single line with a g value of 2.0045 ± 0.0006. The irradiation process gives rise to “cellulose-like” Electron Spin Resonance (ESR) spectrum two lines symmetrical to the central line, at a distance of ca. 3 mT. Irradiation increases the central line and produces two satellite peaks (lines) with an amplitude growing with dose. The stability of the radiation-induced ESR signal at room temperature was studied from a quantitative point of view. The fading study and dose evaluation were pursued for a period of two years analyzing irradiated walnuts samples. The reported curves, describing the fading at different doses, differ only by a multiplicative factor and the attenuation factor (the ratio between the amplitude measured and the amplitude evaluated after irradiation) depends only on the time elapsed following treatment.

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 μg 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.

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.

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.

The aim of the work has two folders: the first is to apply numerical and approximated methods to solve the integral comparing in the thermoluminescence theory, i.e. . The second point is to compare the influence of the two different ways of calculation on the values of the pre-exponential factor.

Food irradiation can be used to increase the microbiological safety and to extend the shelf life of foods. European legislation states that any food or food ingredients must be labelled and every year each Member State, particularly Italy, has to carry out checks at marketing stage. This work reports on the results of analytical controls on 451 foodstuff samples over the period 2006–2011 performed by an Italian accredited laboratory using 4 different screening and confirmatory techniques: PSL, DNA Comet Assay, TL and ESR. A total of 18 samples were found non-compliant: 6 frog legs, 3 clams, 3 cuttlefish, 1 octopus and 1 shrimps from Vietnam; 3 squids, 1 white pepper and 1 chilli tofu from China. Non-compliances are due to both incorrect labelling and irradiation in not approved facilities in extra European/third countries. Check results also showed that among screening methods PSL is the most accurate, simple and practical standard to analyse most of samples (spices, herbs, supplements, mollusks, crustaceans and vegetables) with a low false positive classification (11%) whereas DNA Comet Assay revealed the highest percentage of false positive cases (26%). ESR is the suitable confirmatory method to detect dried fruits and foodstuffs (meat and fish product) containing bone, while TL is the best confirmatory method to detect herbs, spices and supplements, cephalopods, mollusks and crustaceans, besides fresh fruits and vegetables. In conclusion, by comparison with European data, this study suggests more checks on meat products (frog and poultry meats), fish products (cephalopods, mussels and crustacean) spices and supplements especially at import stage from countries where non approved irradiation facilities are operating (e.g. Vietnam and China).

High energy radiation treatment of foodstuff for microbial control and shelf-life extension is being used in many countries. However, for consumer protection and information, the European Union has adopted the Directives 1999/2/EC and 1999/3/EC to harmonize the rules concerning the treatment and trade of irradiated foods in EU countries. Among the validated methods to detect irradiated foods the EU directives also include Electron Paramagnetic Resonance (EPR/ESR) spectroscopy. We describe herein the use of EPR for identification of four species of bivalve mollusks, i.e. brown Venus shells (Callista chione), clams (Tapes semidecussatus), mussels (Mytilus galloprovincialis) and oysters (Ostrea edulis) irradiated with 60Co γ-rays. EPR could definitely identify irradiated seashells due to the presence of long-lived free radicals, primarily CO2−, CO33−, SO2− and SO3− radical anions. The presence of other organic free radicals, believed to originate from conchiolin, a scleroprotein present in the shells, was also ascertained. The use of one of these radicals as a marker for irradiation of brown Venus shells and clams can be envisaged. We also propose a dosimetric protocol for the reconstruction of the administered dose in irradiated oysters.

Treatment of food with ionising radiations in order to increase its shelf-life is largely employed in many countries. Because of restrictions issued by different governments on the use of this technique, in addition to the identification of irradiated foodstuffs, it may be important to determine the radiation dose administered to the foodstuffs. An EPR based protocol to reconstruct the administered dose from samples of irradiated meats (rabbit, pork and duck) within an uncertainty of ±25% is reported. © 2010 Elsevier Ltd.

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.

Irradiation of chestnuts has recently been considered as an alternative treatment to fumigation to reduce the considerable amount of the product normally lost during post-harvest period. The treatment is allowed in countries such as Korea and, in view of a possible extension to European countries, to permit the legal controls as required by the directive 1999/2/EC [ European Parliament and Council Directive, 1999 /2/EC, on the approximation of the laws of the Member States concerning foods and food ingredients treated with ionising radiation. Official Journal of the European Communities. L 66/16 of 13.3.1999] and meet consumer consensus, reliable methods for detecting irradiated chestnuts have to be proposed. The aim of the present work was to test the efficacy of the European Standard EN 13751, EN 1788, EN 1787 and EN 13708 in detecting irradiated chestnuts. For this purpose, six sets of “Montella” chestnuts, a typical Italian variety recognized as a PGI (protected geographical indication), non-irradiated and irradiated at different doses in the 0.1–1 kGy range, were analysed by thermoluminescence (TL), photo-stimulated luminescence (PSL) (screening and calibrated PSL) and ESR techniques. PSL and TL analysis results revealed the low luminescence sensitivity of the chestnuts. Nevertheless, PSL screening data were in the intermediate band above the negative threshold (at all doses except at the lowest one) and TL analysis led to correct positive classifications even at the lowest dose tested (0.15 Gy). On the contrary, no radio-induced ESR signal could be registered with the irradiated samples of chestnut shell or pulp.

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/60 s) 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/60 s), 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.