Bruno Neri

The European Food Safety Authority (EFSA) monitors the presence and concentration of contaminants in food to mitigate health risks. EU legislation sets maximum levels of heavy metals in foods, including cadmium (Cd), lead (Pb), and total Hg (THg) in seafood, due to their toxicity. In the framework of official control, between 2014 and 2023, 5854 seafood samples were collected and 4300 analyses for THg, 3338 for Cd, and 2171 for Pb were performed using Inductively Coupled Plasma Mass Spectrometry (ICP-MS) and cold vapor atomic absorption spectrometry (CVAAS). The aim was to assess the proportion of contaminated foods in the dataset, the concentration of contaminants, and the potential health risks associated with their intake. Of the total samples analyzed, 142 (2.43%) were found to be non-compliant (n.c.). Concentrations exceeding the limits for Cd were primarily detected in cephalopods (n = 17), mainly squids. In contrast, Hg levels exceeded the limits in marine fish (n = 118), notably in swordfish (11.30% of n.c. samples among those analyzed for this species), sharks (6.48%), and tuna species (3.11%). Regarding Pb, only a single bivalve sample was found to exceed the maximum limits. A preliminary assessment of weekly exposure to Hg through swordfish consumption raised concerns about the frequent intake of marine top predators, particularly for vulnerable people.

Bisphenol A (BPA) and some of its analogues are well known as endocrine-disrupting chemicals (EDCs), i.e., compounds that can affect the physiological hormonal pathways in both animals and humans, causing adverse health effects. The intake of these substances through diet represents a public concern, compounded by the scarce data in the literature about contamination levels in food. In the framework of a research project, funded by the Italian Ministry of Health, we determined the contamination levels of BPA and 19 EDCs in the production chain of buffalo milk, analysing feed, drinking water, buffalo milk, and blood sera. Overall, 201 feed, 9 feed additive, 62 drinking water, 46 milk, and 190 blood serum samples were collected from 10 buffalo farms in the Campania region, Southern Italy, between 2019 and 2020, and analysed. Moreover, 15 retail bovine milk samples packaged both in Tetra Pak and in PET were analysed to further evaluate consumers’ exposure to EDCs. The results of our work showed no contamination by EDCs in drinking water samples, whereas in 43% of all of the other samples from the farms at least one bisphenol was detected. The most abundant bisphenol detected was BPA (32% of the samples from the farms and 80% of the retail milk samples), thus proving that this compound is still widely used for plastic production.

(Poly)phosphates are approved as water-preserving and emulsifying agents that improve the appearance and consistency of many food products. The labelling of added (poly)phosphates is essential for protecting vulnerable population groups and to prevent unfair trade practices resulting in economic fraud. The problems with (poly)phosphates’ utilisation concerns both analytical and legislative issues, such as: (1) their straightforward detection; (2) excessive addition altering freshness perception and misleading consumers; (3) uncontrolled usage increasing foodstuff weight; (4) application in products where they are not permitted; and (5) no indication on the label. Bearing all these issues in mind, the main purpose of this study was the quantification and screening of the (poly)phosphates profile in meat, marine and dairy products (160 samples), of which 43 were without declared (poly)phosphate treatment. Analysis was completed by high-performance ion-exchange chromatography either with conductometric detection or coupled to Q-Exactive Orbitrap high-resolution mass spectrometry. Although the (poly)phosphates profiles varied greatly according to species and processing type, the following criteria for detection of illicit treatment were established: high orthophosphate level, quantified short-chain (poly)phosphate anions and the presence of long-chain forms. In conclusion, the instrumental platforms used in this study can be recommended to inspection bodies as reliable methods for the detection of food adulteration with (poly)phosphates.

Silver nanoparticles functionalized with thiolated β-cyclodextrin (CD-SH) were employed for the detection of bisphenols (BPs) A, B, and S by means of surface-enhanced Raman spectroscopy (SERS). The functionalization of Ag nanoparticles with CD-SH leads to an improvement of the sensitivity of the implemented SERS nanosensor. Using a multivariate analysis of the SERS data, the limit of detection of these compounds was estimated at about 10⁻⁷ M, in the range of the tens of ppb. Structural analysis of the CD-SH/BP complex was performed by density functional theory (DFT) calculations. Theoretical results allowed the assignment of key structural vibrational bands related to ring breathing motions and the inter-ring vibrations and pointed out an external interaction due to four hydrogen bonds between the hydroxyl groups of BP and CD located at the external top of the CD cone. DFT calculations allowed also checking the interaction energies of the different molecular species on the Ag surface and testing the effect of the presence of CD-SH on the BPs’ affinity. These findings were in agreement with the experimental evidences that there is not an actual inclusion of BP inside the CD cavity. The SERS sensor and the analysis procedure of data based on partial least square regression proposed here were tested in a real sample consisting of the detection of BPs in milk extracts to validate the detection performance of the SERS sensor.

Coccidiostats are synthetic drugs administered to animals, especially to poultry, to cure coccidiosis. In this paper, we present a selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to analyze residues of five synthetic coccidiostats in eggs: clazuril, diclazuril, robenidine, nicarbazin, toltrazuril and its two metabolites. The extraction efficiency was evaluated by testing several solvents, pH, different volumes and time of extraction. The clean-up procedures were optimized using different solid phase extraction cartridges and different eluants. The chromatographic separation was achieved in reversed phase using a gradient of 0.1% formic acid in water and acetonitrile, whereas the MS detection was performed in negative electrospray ionization (ESI) for all the analytes, except for the robenidine. The developed method has been validated according to Commission Decision 2002/657/CE. The validation parameters, as linearity, precision, recovery, specificity, decision limit (CCα), detection capability (CCβ), and robustness have been determined. The proposed method resulted simple, fast, and suitable for screening and confirmation purposes.