Occurrence of antibiotics in mussels and clams from various FAO areas

Filter feeders, like mussels and clams, are suitable bioindicators of environmental pollution. These shellfish, when destined for human consumption, undergo a depuration step that aims to nullify their pathogenic microorganism load and decrease chemical contamination. Nevertheless, the lack of contamination by drugs may not be guaranteed. Antimicrobials are a class of drugs of particular concern due to the increasing phenomenon of antibiotic resistance. Their use in breeding and aquaculture is a major cause of this. We developed a multiclass method for the HPLC\ue2\u80\u93MS/MS analysis of 29 antimicrobials, validated according to the Commission Decision 2002/657/UE guidelines, and applied it to 50 mussel and 50 clam samples derived from various Food and Agricultural Organisation marine zones. The results obtained, indicate a negligible presence of antibiotics. Just one clam sample showed the presence of oxytetracycline at a concentration slightly higher than the European Union Maximum residue limit set for fish

Distribution of persistent organic pollutants (POPS) IN wild Bluefin tuna (Thunnus thynnus) from different FAO capture zones

Residues of environmental contaminants in food represent a concern in food safety programs. In this study, the distribution of persistent organic pollutants (POPs) were evaluated in 79 tuna samples from FAO areas 51 (Indian Ocean), 71 (Pacific Ocean), 34 (Atlantic Ocean), and 37 (Mediterranean Sea). 6 polychlorinated biphenyls (PCBs), 16 organochlorines (OCs) and 7 polybrominated biphenyl ethers (PBDEs) were selected as representative compounds according to EFSA POPs monitoring guidelines. An analytical method, based on Accelerated Solvent Extraction (ASE), with an "in-line" clean-up step and GC-MS/MS detection, was developed, validated and applied. PCBs were detected in all FAO areas, with a prevalence of 100% for most of them. In the FAO area 37, only, all PBDEs were detected. Only 5 OCs were detected. The results showed that POPs contamination of tuna reflects FAO area contamination; in particular FAO area 37 was the most polluted. Moreover, tuna muscle was an appropriate matrix for monitoring contamination and for obtaining information about food safety

Determination of thyreostats in bovine urine and thyroid glands by HPLC–MS/MS

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 has 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\u2013liquid 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\u2013104 % 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 \u3bcg L 121 and 10 \u3bcg kg 121, respectively. In urine, the limits of decision ranged from 6.9 to 7.3 \u3bcg L 121, and the capacities of detection ranged from 8.5 to 9.7 \u3bcg L 121, while in thyroid glands these values varied from 6.6 \u3bcg kg 121 to 7.4 \u3bcg kg 121 and from 8.0 \u3bcg g 121 to 9.7 \u3bcg kg 121, respectively. The results obtained show that the methods described are suitable for the direct detection of thyreostats in bovine urine and thyroid glands

Synthesis and characterization of 4-hydroxy-2-nonenal derivatives for gas chromatographic analysis with electron capture detection (GC-ECD)

4-Hydroxy-2-nonenal (HNE) has been prepared from the corresponding dimethylacetal (HNE-DMA), in turn synthesized by a conventional approach with a few modifications of the experimental protocol and some improvements in the purification of the final product. In order to exploit the sensitivity of gas-chromatography with electron capture detector (GC-ECD) in the analysis of HNE derivatives, reaction of HNE with 2,4,6-trichlophenylhydrazine (TCPH) and 3,5-dichlorophenylhydrazine (DCPH) was tested. Reaction with TCPH afforded a mixture of products, whereas with DCPH a single major product was formed that was prepared on a millimolar scale and purified. 1H-NMR analysis established that the derivative of HNE with DCPH is HNE 3,6-dichlorophenylhydrazone, that can be used as standard for GC-ECD analysis

Detection of perfluoroalkyl acids and sulphonates in Italian eel samples by HPLC-HRMS Orbitrap

Perfluoroalkyl substances (PFASs) contain one or more carbon-bound hydrogens substituted by fluorine. Since the 1950s, these compounds have been used to manufacture fat- and water-resistant fabrics, paper and food containers, and to produce photographic films, firefighting foams, detergents and insecticides. The widespread use and global distribution of PFASs, have led to their accumulation in the environment. Food, particularly fish and other seafood, is considered the main route of human exposure to PFASs. Consequently, the European Food Safety Authority (EFSA) recommends that more data be collected, to build a database on the contamination levels of the individual PFASs in food, to evaluate a reliable chronic risk to the European consumers. This requires high-sensitivity analytical methods, to increase the number of quantifiable samples and, thereby, improve the credibility of exposure assessments. In this context, the aim of the present research is to develop and validate a sensitive and specific method based on high-performance liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) analysis, to monitor the presence of 16 PFASs in Italian eels (Anguilla anguilla) from the Italian Lake Garda. The detection limits (CCa) and detection capability (CCb) in the order of pg g1 , the recoveries between 80 and 101% and the other validation parameters fulfilled the requirements of Commission Decision 657/ 2002/EC. The identification and quantification of PFASs, up to 11 in the same sample, showed a similar distribution among 90 eels. Perfluorooctane sulphonic acid (PFOS) and perfluorobutanoic acid (PFBA) were the analytes more frequently found in the eel samples (94 and 82%, respectively)

Secondary Metabolite Profile, Antioxidant Capacity, and Mosquito Repellent Activity of Bixa orellana from Brazilian Amazon Region

The Brazilian flora was widely used as source of food and natural remedies to treat various diseases. Bixa orellana L. (Bixaceae), also known as annatto, uruc\uf9, or achiote, is a symbol for the Amazonian tribes that traditionally use its seeds as coloured ink to paint their bodies for religious ceremonies. The aim of this study was to investigate the volatile organic compounds (VOCs) profile of B. orellana fresh fruits (in vivo sampled), dried seeds, wood, bark, and leaves analyzed with Headspace solid-phase microextraction coupled with gas chromatography and mass spectrometry. A screening on phenolic content (the Folin-Ciocalteu assay) and antiradical activity (DPPH assay) of seeds was also conducted. In addition, the repellent properties of seed extracts against Aedes aegypti L. were investigated. Volatile compounds detected in B. orellana samples consisted mainly of sesquiterpenes, monoterpenes, and arenes: \u3b1-humulene is the major volatile compound present in seed extracts followed by D-germacrene, \u3b3-elemene, and caryophyllene. B. orellana proved to be a good source of antioxidants. Preliminary data on repellency against A. aegypti of three different dried seed extracts (hexane, ethanol, and ethanol/water) indicated a significant skin protection activity. A protection of 90% and 73% for hexane and ethanol/water extracts was recorded

Determination of Volatile Organic Compounds (VOCs) from wrapping films and wrapped PDO Italian cheeses by using HS-SPME and GC/MS

Nowadays food wrapping assures attractive presentation and simplifies self-service shopping. Polyvinylchloride (PVC)- And polyethylene (PE)-based cling-films are widely used worldwide for wrapping cheeses. For this purpose, films used in retail possess suitable technical properties such as clinginess and unrolling capacity, that are achieved by using specific plasticizers during their manufacturing process. In the present study, the main VOCs of three cling-films (either PVC-based or PE-based) for retail use were characterized by means of Solid-Phase Micro-Extraction and GC/MS. In addition, the effects of cling film type and contact time on the migration of VOCs from the films to four different PDO Italian cheeses during cold storage under light or dark were also investigated. Among the VOCs isolated from cling-films, PVC released 2-ethylhexanol and triacetin. These compounds can likely be considered as a "non-intentionally added substance". These same compounds were also detected in cheeses wrapped in PVC films with the highest concentration found after 20 days storage. The PE cling-film was shown to possess a simpler VOC profile, lacking some molecules peculiar to PVC films. The same conclusions can be drawn for cheeses wrapped in the PE cling-film. Other VOCs found in wrapped cheeses were likely to have been released either by direct transfer from the materials used for the manufacture of cling-films or from contamination of the films. Overall, HS-SPME is shown to be a rapid and solvent free technique to screen the VOCs profile of cling-films, and to detect VOCs migration from cling-films to cheese under real retail storage conditions

Different behaviour of 3-nitrotyrosine and tyrosine toward perfluorinated reagents suitable for the one-step preparation of volatile derivatives

With the view of developing a gas-chromatographic (GC) determination of the 3-nitrotyrosine (NY)/tyrosine (Y) ratio as a marker of nitro-oxidative stress, different reagents were tested with the objective of obtaining a single volatile fluorinated product for each amino acid in a one-step derivatisation procedure. The heptafluorobutyric anhydride (HFBA)/heptafluorobutanol (HFBOH) mixture proved unsuccessful for the simultaneous analysis of NY and Y. The reaction with different chloroformates, isobutyl chlorofomate (iBuCF) and ethyl chloroformate (EtCF) in the presence of different perfluorinated alcohols, such as trifluoroethanol (TFEOH) and HFBOH, was investigated. A combination EtCF/fluorinated alcohols yielded derivatives of NY and Y as single peaks suitable for the GC determination of the NY/Y ratio. The different behaviours of the two amino acids in the employed reaction mixtures and the parameters influencing the results are discussed

Food safety in food services in lombardy : proposal for an inspection-scoring model

The purpose of this study was to elaborate a checklist with an inspection scoring system at national level in order to assess compliance with sanitary hygiene requirements of food services. The inspection scoring system was elaborated taking into account the guidelines drawn up by NYC Department of Food Safety and Mental Hygiene. Moreover the checklist was used simultaneously with the standard inspection protocol adopted by Servizio Igiene Alimenti Nutrizione (Servizio Igiene Alimenti Nutrizione - Ss. I.A.N) and defined by D.G.R 6 March 2017 \u2013 n. X/6299 Lombardy Region. Ss. I.A.N protocol consists of a qualitative response according to which we have generated a new protocol with three different grading: A, B and C. The designed checklist was divided into 17 sections. Each section corresponds to prerequisites to be verified during the inspection. Every section includes the type of conformity to check and the type of violation: critical or general. Moreover, the failure to respect the expected compliance generates 4 severity levels that correspond to score classes. A total of 7 food services were checked with the two different inspection methods. The checklist results generated a food safety score for each food service that ranged from 0.0 (no flaws observed) to 187.2, and generates three grading class: A (0.0-28.0); B (29.0 - 70.0) and C (>71.00). The results from the Ss. I. A. N grading method and the checklist show positive correlation (r=0.94, P>0.01) suggesting that the methods are comparable. Moreover, our scoring checklist is an easy and unique method compared to standard and allows also managers to perform effective surveillance programs in food service