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A fast, easy, and cheap method for the simultaneous determination and quantification of aflatoxins (B1, B2, G1, G2), T-2 and HT-2 toxins, and fumonisins (B1, B2) in cereal-derived products was developed. This method involved a quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction coupled with liquid chromatography-tandem mass spectrometry. The method validation was performed by analyzing samples spiked at four levels, and the recoveries ranged from 83.6 to 102.9%, whereas the maximum values of repeatability and within-laboratory reproducibility were 14.3 and 15.7% following the performance criteria set by the European legislation. The method was then applied for the analysis of 21 cereal-derived products purchased on the Italian market, which were correctly packaged and labeled as intended for human consumption. The co-occurrence of more than one mycotoxin in the analyzed samples could represent a risk for consumers, and the described method could be a valid alternative for their simultaneous detection in the framework of official control. Graphical Abstract ᅟ.

In this study, the development and validation of a multiresidue method for the detection of 11 quinolones (marbofloxacin, norfloxacin, ciprofloxacin, danofloxacin, lomefloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid, nalidixic acid, flumequine) in muscle and eggs were reported. The method involved an extraction with a methanol/metaphosphoric acid mixture and a clean up by Oasis hydrophilic-lipophilic balance (HLB) cartridge. The validation was performed according to the Commission Decision 2002/657/EC. Linearity, specificity, decision limit (CCα), detection capability (CCβ), recovery, precision (repeatability and within-laboratory reproducibility), and ruggedness were determined. Depending on the analytes, CCα and CCβ ranged from 113 to 234 μg/kg and from 126 to 282 μg/kg in muscle samples, whereas in eggs, these parameters were between 5.6 and 7.4 μg/kg and between 6.1 and 9.8 μg/kg, respectively. In both the examined matrices, the recovery values were always higher than 90 % and precision, calculated as relative standard deviation, was equal to or lower than 16 % for repeatability and 23 % for within-laboratory reproducibility. The described method can be considered adequate for the simultaneous determination and quantification of quinolones in the tested food matrices.

In this study samples of feedstuffs were collected from different feed mills and animal farms located in central Italy and analyzed for ionophore coccidiostat residues at carry-over levels by liquid chromatography-mass spectrometry. Since unavoidable cross-contamination of feedstuffs may occur during their production as well as distribution and storage, the collection of samples covered all these different stages. Residues of lasalocid, monensin, salinomycin and maduramicin were detected in 32.4% of samples, both at production and storage level. The maximum content for unavoidable carry-over set by Regulation (EU) No 574/2011 was exceeded in 11.3% of samples. The variability of the results highlighted the different approach of each investigated feed business operator to avoid any cross-contamination in non-target feed. The method developed in this study can be able to detect ionophore coccidiostats at low concentrations consequent to carry-over.

Histamine formation in Sardina pilchardus and Engraulis encrasicolus as a function of storage temperature was studied. Fish were caught off the Adriatic Coast and were carried immediately to the laboratory. A portion of dorsal muscle from each fish was soon analyzed, while two other portions were examined after storage at two different temperatures (25 and 4C) for 24 and 72 h, respectively. The analyses were carried out by high‐performance liquid chromatography (HPLC)‐UV and confirmed by HPLC‐diode array detector. Histamine concentrations were always higher than the European Community admissible levels in samples stored at 25C. In fish stored at 4C, histamine was detected only in E. encrasicolus. PRACTICAL APPLICATIONS Time experiments were conducted to quantify the histamine formation in scombroid species at two different temperatures. The first assay (24 h, 25C) could reproduce the modality of sale adopted by fishermen or retailers in summer on the one hand, and the maintenance at ambient temperature of semipreserved sardines or anchovies during salting and ripening on the other hand. The second experiment (72 h, 4C) was based on the domestic cold preservation of fish before the consumption, which sometimes occurs some days after purchasing. Even if ice storage is recommended, time/temperature abuse conditions often occur in the fish merchandising chain. The results of this research showed that high histamine concentrations could be found in the analyzed species not only at an abused temperature, but also at a common storage temperature of fish at home.

Samples of flour derived from an organic wheat seed cultivated in the region Abruzzo (Central Italy) were examined for the detection of aflatoxins, deoxynivalenol, ochratoxin A and zearalenone after storage in the presence of oxygen or under vacuum, for one year. They were analysed by high-performance liquid chromatography with fluorescence detection for aflatoxins, ochratoxin A and zearalenone and with diode array detector for deoxynivalenol. An immunoaffinity column clean-up was applied for all the compounds, except for aflatoxin determination, which required a solid-phase extraction. Recoveries (range: 76-107%) and within-laboratory reproducibility (RSD% < 10.3) met the performance criteria of Commission Regulation (EU) No. 519/2014 amending Commission Regulation (EC) No. 401/2006 for the detection of mycotoxins in foodstuffs. Analytes were below the detection limit of the method, and this result was probably due to the quality of organic seed and good agricultural practices performed for the prevention of mycotoxin formation.

Residues of nonionophoric coccidiostats at carryover concentrations in feedstuffs collected from feed mills or animal farms in central Italy were detected as part of the official controls carried out from 2011 through 2016. The 118 samples were collected on the production line or during feed distribution and storage to determine the sampling sites at major risk of cross-contamination. For determination of nonionophoric coccidiostats, a fast, easy, and cheap method was developed and validated. Feed samples were extracted with acetonitrile-methanol and directly injected for liquid chromatography with tandem mass spectrometry. A total of 24 samples (20.3%) were positive, but only 5 (4.2%) of these samples exceeded the maximum limit set by European legislation. Most of the positive samples were collected from a batch of feed produced immediately following processing of another batch to which the coccidiostat robenidine had been added.

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