Bee products, such as honey, are widely consumed as food and consumer interest is currently oriented towards organic foods. Regarding this, the European Commission establishes that the qualification of organic honey and other beekeeping products as being from organic production is closely bound with the characteristics of hive treatments as well as the quality of the environment. Agricultural contamination with pesticides is a challenging problem that needs to be fully addressed, in particular in the field of organic production systems. In this study, the occurrence of different classes of contaminants selected as representative of potential contamination sources were investigated in 59 organic honeys: organochlorines, OCs; organophosphates, OPs; polychlorobiphenyls, PCBs and polybromodiphenylethers, PBDEs. A method based on Accelerated Solvent Extraction with "in line" clean-up and GC-MS/MS detection was developed to detect contaminants. Residues of many pesticides were found in most of the samples investigated. The majority of honey samples contained at least one of the pesticides, even if their concentrations were found to be lower than its MRL. Diazinon, Mevinphos, Coumaphos, Chlorpyrifos and Quinoxyfen were the residues frequently detected in samples coming from the apple and citrus orchard areas. Furthermore, the results of the present study show that the presence of the residue in organic honey may also be affected by the geographical area (e.g. the presence of an agricultural system) confirming honey bee and beehive matrices as appropriate sentinels for monitoring contamination in the environment. The optimised method proved to be simple and rapid, requiring small sample sizes and minimising solvent consumption, due to the ASE having an "in line" clean-up step.

Reviewing the presence of contaminant residues is important both for food safety and for monitoring of environmental pollution. Here, the occurrence of 6 polychlorinated biphenyls (PCBs), 15 organochlorine pesticides (OCPs), 7 polybrominated diphenyl ethers (PBDEs), 4 polycyclic aromatic hydrocarbons (PAHs) and 17 perfluoroalkyl substances (PFASs) was evaluated in mussels and clams. A liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) and an innovative QuEChERS extraction followed by gas chromatography-tandem mass spectrometry (GC-MS/MS) methods were developed, validated and applied. We demonstrate good linearity, repeatability and accuracy of these methods, confirming that they are suitable for the analyses of mollusc samples. The prevalence of PCBs, OCPs and PAHs was higher in mussels than in clams. For PFASs, contamination was higher in clams than in mussels. The samples were all compliant with the regulations, and, for the compounds without legislative limits, a risk assessment confirmed that the values were lower than the tolerable intakes.

24Residues of environmental contaminants in food represent a concern in food safety 25 programs. In this study, the distribution of persistent organic pollutants (POPs) were

The worldwide loss of honeybee colonies may be due to their exposure to several contaminants (i.e., pesticides); such contamination may also have impacts on consumers' health. Therefore, it is essential to develop quick and new methods to detect several pesticide residues in honey samples. In this study, the effectiveness of accelerated solvent extraction (ASE) was compared with QuEChERS methods for the analysis of 53 pesticides in organic honey by gas chromatography-triple quadrupole mass spectrometry. Two simple and rapid ASE methods with 'in-line' clean-up were optimised and then compared with QuEChERS. Hexane-ethyl acetate (Hex:EtAc) and Florisil were chosen as extraction solvent and retainer for the first ASE method respectively; acetonitrile and a primary-secondary amine phase (ACN-PSA) were selected for the second ASE method. The methods were validated according to the European Union SANTE/11945/2015 guidelines. The validation parameters showed that QuEChERS and ASE with PSA as retainer had better repeatability than ASE with Hex:EtAc and Florisil. In particular, QuEChERS and ASE (ACN-PSA) showed good recovery, according to the SANTE criteria, for the majority of investigated pesticides. Conversely, when ASE with Hex:EtAc and Florisil was used as the retainer, several compounds showed recoveries lower than the acceptable value of 70%. The ASE in-line method was finally applied to evaluate pesticide concentration in organic honey samples.

Abstract:Abstract The use of thyreostats in livestock is strictly forbidden by European legislation since 1981. The investigation of thyreostats is commonly performed by their detection as derivatives with 3-iodobenzylbromide. Although it leads advantages, the derivatisation procedure can generally cause a decrease in analyte concentrations. With the aim of simplifying the analysis of five thyreostats in both bovine urine and in thyroid glands, two methods were developed without the derivatisation step. Salting-out assisted liquid-liquid extraction was carried out for both matrices, followed by high-performance liquid chromatography coupled with triple-quadrupole mass spectrometry analysis. The methods were validated in agreement with the guidelines of Commission Decision 2002/657/EC. For all the thyreostats evaluated, satisfactory results were achieved; the recovery was within 96% to 104% for both the matrices, while precision (coefficient of variation) was less than 20% for urine and 21% for thyroid glands. The limits of decision and capacities of detection for all the compounds were lower than the recommended values of 10 μg L-¹ and 10 μg kg-¹, respectively. In urine, the limits of decision ranged from 6.9 to 7.3 μg L-¹, and the capacities of detection ranged from 8.5 to 9.7 μg L-¹, while in thyroid glands these values varied from 6.6 μg kg-¹ to 7.4 μg kg-¹ and from 8.0 μg g-¹ to 9.7 μg kg-¹, respectively. The results obtained show that the methods described are suitable for the direct detection of thyreostats in bovine urine and thyroid glands.

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The debate about the origin of prednisolone in animal organisms has lasted for 5 years. Bovine species have been the most studied, but studies on humans and horses are also present in the literature. Even if prednisolone in pigs does not yet represent a problem for control agencies, interest has recently increased with regard to this species. To date, there has been just a single study in the literature about this topic, performed on 10 sows treated with prednisolone or a synthetic analogue of adrenocorticotropic hormone. We therefore initiated a study on 80 pigs, a number considered representative in relation to the expected frequency (prevalence) of prednisolone detection in urine collected at slaughter. Prednisolone was detected in urine both at the farm and at the slaughterhouse, with a concentration and frequency higher at slaughter. The presence of prednisolone was also studied in the adrenal glands, where the corticosteroids are produced in response to stress, and it was detected in 89% of the samples. These results, together with the similar behaviours of prednisolone and cortisol, i.e. a mutual rise in the two corticosteroids in urine collected at the slaughterhouse and the correlation between the concentrations of the two corticosteroids in the adrenal glands, seem to indicate an endogenous origin of prednisolone in pigs.

No abstract