ketoprofen, naproxen and venlafaxine were the compounds most frequently found. In the highlight of these results, the number of analytes was increased up to around 50. A lot of antibiotic compounds were added to the target list as they were considered "priority pharmaceuticals" due to their more potential hazardous effects in the aquatic environment. Data obtained during the second monitoring programme (spring and autumn) corroborated the results from the first one (summer and winter). Analgesics and anti-inflammatories, lipid regulators together with quinolone and macrolide antibiotics were the most abundant pharmaceuticals.Similar median concentrations were found over the year and seasonal variation was not clearly observed. The removal efficiency of pharmaceuticals in the wastewater treatment plants was roughly evaluated. Our results indicated that elimination of most of the selected compounds occurred during the treatment process of influent wastewater, although it was incomplete.

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Plant ingredients and processed animal proteins (PAP) are suitable alternative feedstuffs for fish feeds in aquaculture practice, although their use can introduce contaminants that are not previously associated with marine salmon and gilthead sea bream farming. Mycotoxins are well known natural contaminants in plant feed material, although they also could be present on PAPs after fungi growth during storage. The present study surveyed commercially available plant ingredients (19) and PAP (19) for a wide range of mycotoxins (18) according to the EU regulations. PAP showed only minor levels of ochratoxin A and fumonisin B1 and the mycotoxin carry-over from feeds to fillets of farmed Atlantic salmon and gilthead sea bream (two main species of European aquaculture) was performed with plant ingredient based diets. Deoxynivalenol was the most prevalent mycotoxin in wheat, wheat gluten and corn gluten cereals with levels ranging from 17 to 814 and μg kg(-1), followed by fumonisins in corn products (range 11.1-4901 μg kg(-1) for fumonisin B1+B2+B3). Overall mycotoxin levels in fish feeds reflected the feed ingredient composition and the level of contaminant in each feed ingredient. In all cases the studied ingredients and feeds showed levels of mycotoxins below maximum residue limits established by the Commission Recommendation 2006/576/EC. Following these guidelines no mycotoxin carry-over was found from feeds to edible fillets of salmonids and a typically marine fish, such as gilthead sea bream. As far we know, this is the first report of mycotoxin surveillance in farmed fish species.

This article describes the development, validation and application of a rapid screening method for the detection and identification of undesirable organic compounds in aquaculture products. A generic sample treatment was applied without any purification or preconcentration step. After extracting the samples with acetonitrile/water 80:20 (0.1% formic acid), the extracts were centrifuged and directly injected in the LC-HRMS system, consisting of ultra-high performance liquid chromatography coupled to hybrid quadrupole time-of-flight mass spectrometry (UHPLC-QTOF MS). A qualitative validation was carried out for over 70 representative compounds, including antibiotics, pesticides and mycotoxins, in fish feed and fish fillets spiked at 20 µg/Kg and 100 µg/Kg. At the highest level, the great majority of compounds were detected (using the most abundant ion, typically the protonated molecule) and unequivocally identified (based on the presence of two accurate-mass measured ions). At the 20 µg/Kg level, many contaminants could already be detected although identification using two ions was not fully reached for some of them, mainly in fish feed due to the complexity of this matrix. Subsequent application of this screening methodology to aquaculture samples made it possible to find several compounds from the target list, such as the antibiotic ciprofloxacin, the insecticide pirimiphos-methyl and the mycotoxins fumonisin B2 and zearalenone. A retrospective analysis of accurate-mass full-spectrum acquisition data provided by QTOF MS was also made, without neither reprocessing nor injecting the samples. This allowed the detection and tentative identification of other organic undesirables different than those included in the validated list.

Cita bibliográfica / Cita bibliogràfica (ISO 690):NÁCHER-MESTRE, Jaime, et al. Screening of pesticides and polycyclic aromatic hydrocarbons in feeds and fish tissues by gas chromatography coupled to high-resolution mass spectrometry using atmospheric pressure chemical ionization.

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24The aim of the present work was to analyze the effect of partial and total replacement of fish 25 oil (FO) by a blend of vegetable oils on the health and antioxidant status of gilthead sea 26 bream (Sparus aurata L.) fed primarily plant-protein based diets. The study included 27 measurements of feed-borne contaminants, gene expression analyses of detoxifying and 28 antioxidant pathways and measures of antioxidant and innate immune descriptors. 29Polybrominated diphenyl ethers (PBDEs) were almost undetectable in all diets, and the 30 loading-charges of polychlorinated biphenyls (PCBs), dioxin-like PCBs, organochlorine 31 pesticides (OCs), and polycyclic aromatic hydrocarbons (PAHs) were at trace levels 32 decreasing their concentrations according to the level of FO replacement with vegetable oils 33 (0%, 33%, 66%, 100%). Hepatic detoxifying pathways were down regulated by FO 34 replacement, and the hepatic transcription of cytochrome P450 1A1 and aryl hydrocarbon 35 receptor 1 was significantly reduced in fish fed the 100% vegetal oil diet. Dietary 36 intervention did not alter the hepatic expression of the recycling glutathione reductase, 37 whereas glutathione peroxidase-1 and phospholipid glutathione peroxidase were either down 38 or up-regulated by the total FO replacement. This suggests that vegetable oils prime the in 39 situ repair of peroxidized phospholipids rather than the increased turnover of membrane 40 phospholipids from the undamaged pool of cytosolic free fatty acids. The hepatic expression 41 of non-enzymatic antioxidants (metallothionein, glucose regulated protein 75) was down 42 regulated in fish fed 66% and 100% vegetable oil diets. Hepatic glutathione levels and total 43 plasma antioxidant capacity were also lowest in fish fed high levels of vegetable oils, but the 44 concurrent increase in the GSH/GSSG ratio was interpreted as an index of reduced oxidative 45 stress. This redox balance agrees with the enhanced respiratory burst of blood leucocytes 46 after PMA stimulation in fish feed the 100% vegetable oil. Total plasma peroxidases and 47 plasma alternative complement pathway were not affected by dietary treatment, whereas 48 plasma lysozyme was significantly decreased in fish fed the 66% vegetable oil diet. Taken 49 together, the results suggest that the health and the antioxidant status of gilthead sea bream 50 was not damaged by high levels of FO replacement in eco-friendly diets, but both the 51 scavenging and production of reactive oxygen species were modulated in concert by complex 52 and nutritionally-mediated readjustments. 53Key words: fish oil, vegetal oil, plant proteins, aryl hydrocarbon receptors, cytochrome 54 P450 1A1, glucose regulated protein 75, metallothionein, glutathione, alternative 55 complement pathway, lysozyme, peroxidases, ROS production. 56 57 3