TY - JOUR A1 - Westwood, S. A1 - Josephs, R. A1 - Choteau, T. A1 - Daireaux, A. A1 - Mesquida, C. A1 - Wielgosz, R. A1 - Rosso, A. A1 - de Arechavaleta, M.R. A1 - Davies, S. A1 - Wang, H. A1 - do Rego, E.C.P. A1 - Rodrigues, J.M. A1 - de Freitas Guimaraes, E. A1 - Sousa, M.V.B. A1 - Monteiro, T.M. A1 - das Neves Valente, L.A. A1 - Violante, F.G.M. A1 - Almeida, R. R. R. A1 - Quaresma, M.C.B. A1 - Nogueira, R. A1 - Windust, A. A1 - Dai, X. A1 - Li, X. A1 - Zhang, W. A1 - Li, M. A1 - Shao, M. A1 - Wei, C. A1 - Wong, S.-K. A1 - Cabillic, J. A1 - Gantois, F. A1 - Philipp, Rosemarie A1 - Pfeifer, Dietmar A1 - Hein, Sebastian A1 - Klyk-Seitz, Urszula-Anna A1 - Ishikawa, K. A1 - Castro, E. A1 - Gonzalez, N. A1 - Krylov, A. A1 - Lin, T.T. A1 - Kooi, L.T. A1 - Fernandes-Whaley, M. A1 - Prévoo, D. A1 - Archer, M. A1 - Visser, R. A1 - Nlhapo, N. A1 - de Vos, B. A1 - Ahn, S. A1 - Pookrod, P. A1 - Wiangnon, K. A1 - Sudsiri, N. A1 - Muaksang, K. A1 - Cherdchu, C. A1 - Gören, A.C. A1 - Bilsel, M. A1 - LeGoff, T. A1 - Bearden, D. A1 - Bedner, M. A1 - Duewer, D. A1 - Hancock, D. A1 - Lang, B. A1 - Lippa, K. A1 - Schantz, M. A1 - Sieber, j. T1 - Final report on key comparison CCQM-K55.b (aldrin): An international comparison of mass friction purity assignment of aldrin N2 - Under the auspices of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) a key comparison, CCQM K55.b, was coordinated by the Bureau International des Poids et Mesures (BIPM) in 2010/2011. Nineteen national measurement institutes and the BIPM participated. Participants were required to assign the mass fraction of aldrin present as the main component in the comparison sample for CCQM-K55.b which consisted of technical grade aldrin obtained from the National Measurement Institute Australia that had been subject to serial recrystallization and drying prior to sub-division into the units supplied for the comparison. Aldrin was selected to be representative of the performance of a laboratory's measurement capability for the purity assignment of organic compounds of medium structural complexity [molar mass range 300 Da to 500 Da] and low polarity (pKOW < -2) for which related structure impurities can be quantified by capillary gas phase chromatography (GC). The key comparison reference value (KCRV) for the aldrin content of the material was 950.8 mg/g with a combined standard uncertainty of 0.85 mg/g. The KCRV was assigned by combination of KCRVs assigned by consensus from participant results for each orthogonal impurity class. The relative expanded uncertainties reported by laboratories having results consistent with the KCRV ranged from 0.3% to 0.6% using a mass balance approach and 0.5% to 1% using a qNMR method. The major analytical challenge posed by the material proved to be the detection and quantification of a significant amount of oligomeric organic material within the sample and most participants relying on a mass balance approach displayed a positive bias relative to the KCRV (overestimation of aldrin content) in excess of 10 mg/g due to not having adequate procedures in place to detect and quantify the non-volatile content–specifically the non-volatile organics content–of the comparison sample. There was in general excellent agreement between participants in the identification and the quantification of the total and individual related structure impurities, water content and the residual solvent content of the sample. The comparison demonstrated the utility of 1H NMR as an independent method for quantitative analysis of high purity compounds. In discussion of the participant results it was noted that while several had access to qNMR estimates for the aldrin content that were inconsistent with their mass balance determination they decided to accept the mass balance result and assumed a hidden bias in their NMR data. By contrast, laboratories that placed greater confidence in their qNMR result were able to resolve the discrepancy through additional studies that provided evidence of the presence of non-volatile organic impurity at the requisite level to bring their mass balance and qNMR estimates into agreement. PY - 2012 DO - https://doi.org/10.1088/0026-1394/49/1A/08014 SN - 0026-1394 SN - 1681-7575 VL - 49 IS - CCQM-K55.b Final Report October 2012 SP - 1 EP - 41 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-26831 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Santos de Freitas, M. A1 - Araghi, R. R. A1 - Brandenburg, E. A1 - Leiterer, Jork A1 - Emmerling, Franziska A1 - Folmert, K. A1 - Gerling-Driessen, U. I. M. A1 - Bardiaux, B. A1 - Böttcher, C. A1 - Pagel, K. A1 - Diehl, A. A1 - v. Berlepsch, H. A1 - Oschkinat, H. A1 - Koksch, B. T1 - The protofilament architecture of a de novo designed coiled coil-based amyloidogenic peptide N2 - Amyloid fibrils are polymers formed by proteins under specific conditions and in many cases they are related to pathogenesis, such as Parkinson’s and Alzheimer’s diseases. Their hallmark is the presence of a β-sheet structure. High resolution structural data on these systems as well as information gathered from multiple complementary analytical techniques is needed, from both a fundamental and a pharmaceutical perspective. Here, a previously reported de novo designed, pH-switchable coiled coil-based peptide that undergoes structural transitions resulting in fibril formation under physiological conditions has been exhaustively characterized by transmission electron microscopy (TEM), cryo-TEM, atomic force microscopy (AFM), wide-angle X-ray scattering (WAXS) and solid-state NMR (ssNMR). Overall, a unique 2-dimensional carpet-like assembly composed of large coexisiting ribbon-like, tubular and funnel-like structures with a clearly resolved protofilament substructure is observed. Whereas electron microscopy and scattering data point somewhat more to a hairpin model of β-fibrils, ssNMR data obtained from samples with selectively labelled peptides are in agreement with both, hairpin structures and linear arrangements. KW - Amyloid KW - Elektronenmikroskopie PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-458713 UR - https://www.sciencedirect.com/science/article/pii/S1047847718301333 DO - https://doi.org/10.1016/j.jsb.2018.05.009 SN - 1047-8477 VL - 203 IS - 3 SP - 263 EP - 272 PB - Elsevier AN - OPUS4-45871 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Almeida, Ângela A1 - Calisto, V. A1 - Esteves, V.I. A1 - Schneider, Rudolf A1 - Soares, A.M.V.M. A1 - Figueira, E. A1 - Freitas, R. T1 - Presence of the pharmaceutical drug carbamazepine in coastal systems: Effects on bivalves N2 - Carbamazepine (CBZ), an antiepileptic drug, is one of the most commonly detected pharmaceutical drugs in aquatic ecosystems, and is used as a marker of urban pollution. Since CBZ is designed to exert a biological effect, when it reaches aquatic environment high probability exist for toxic effects on non-target organisms. The present study evaluated the acute toxicity of environmentally relevant concentrations of CBZ (0.00, 0.03, 0.30, 3.00, 9.00 µg/L) in the edible clams Venerupis decussata (a native species) and Venerupis philippinarum (an invasive species) collected from the Ria de Aveiro. The effects on both species were assessed through the use of a battery of biomarkers mainly related with health status and oxidative stress. Furthermore, in this work an alternative and promising tool, the direct competitive immunoassay ELISA, for the direct CBZ quantification in clam's tissues, was applied. The results of the present work showed that CBZ in clam's tissues increased with the exposure concentration and V. decussata gave slightly higher values than V. philippinarum. Although the clams accumulated lower levels of CBZ than the concentration of exposure, these concentrations were enough to impair the health status and induce oxidative stress. However, a different response to CBZ was observed in the two species. While in V. philippinarum the lipid peroxidation levels increased at the highest CBZ concentration (9.00 µg/L), in V. decussata a significant decrease was seen. Moreover, glutathionse S-transferase activity was stimulated in V. decussata and decreased in V. philippinarum. Nevertheless, an induction of glutathione reductase, superoxide dismutase and cytochrome P450 3A4 activities was found in both species as a result of the exposure. The results indicate that, probably, V. philippinarum have a less efficient antioxidant system than V. decussata, and are therefore less capable to neutralize oxidative stress and consequently more sensitive to CBZ. The risk quotient determined for the Ria de Aveiro was higher than 1 indicating that a ecotoxicological risk is suspected. Furthermore, bioaccumulation of CBZ in clams should be taken into consideration since this chemical might be transferred along the food chain and affect non-target organisms. KW - Acute toxicity KW - Biomarkers KW - ELISA immunoassay KW - Pharmaceuticals KW - Clams KW - Carbamazepin KW - Toxikologie KW - Toxicology PY - 2014 DO - https://doi.org/10.1016/j.aquatox.2014.08.002 SN - 0166-445x SN - 1879-1514 VL - 156 SP - 74 EP - 87 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-31336 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pieres, A. A1 - Almeida, Ângela A1 - Correia, J. A1 - Calisto, V. A1 - Schneider, Rudolf A1 - Esteves, V. I. A1 - Soares, A. M. V. M. A1 - Figueira, E. A1 - Freitas, R. T1 - Long-term exposure to caffeine and carbamazepine: Impacts on the regenerative capacity of the polychaete Diopatra neapolitana N2 - The toxicity induced in non-target organisms by pharmaceutical drugs has been the focus of several studies. In the aquatic environment, most of the studies have been devoted to fish and bivalves, while little is known on the impacts induced in polychaetes. The present study evaluated the impacts of carbamazepine and caffeine on the regenerative capacity of Diopatra neapolitana, a polychaete species with high ecological and economic relevance. Under laboratory controlled conditions polychaetes were exposed, during 28 days, to carbamazepine (Ctl-0.0; 0.3; 3.0; 6.0; 9.0 mg/L) and caffeine (Ctl-0.0; 0.5; 3.0; 18.0 mg/L). During the experiment, at days 11, 18, 25, 32, 39 and 46 after amputation, for each specimen, the percentage of the body width regenerated was determined and the number of new segments was counted. The regenerative capacity was assessed considering the number of days needed to achieve full regeneration and the total number of new segments. The obtained results revealed that with the increase of drugs concentrations organisms regenerated less new segments and took longer to completely regenerate. KW - Diopatra neapolitana KW - Pollution KW - Pharmaceutical drugs KW - Regenerative capacity PY - 2016 DO - https://doi.org/10.1016/j.chemosphere.2015.12.035 SN - 0045-6535 VL - 146 SP - 565 EP - 573 PB - Elsevier AN - OPUS4-38497 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Freitas, R. A1 - Almeida, Ângela A1 - Calisto, V. A1 - Velez, C. A1 - Moreira, A. A1 - Schneider, Rudolf A1 - Esteves, V. I. A1 - Wrona, F. J. A1 - Figueira, E. A1 - Soares, A. M. V. M. T1 - The impacts of pharmaceutical drugs under ocean acidification: Newdata on single and combined long-term effects of carbamazepine on Scrobicularia plana N2 - Ocean acidification and increasing discharges of pharmaceutical contaminants into aquatic systems are among key and/or emerging drivers of environmental change affecting marine ecosystems. A growing body of evidence demonstrates that ocean acidification can have direct and indirect impacts on marine organisms although combined effects with other stressors, namely with pharmaceuticals, have received very little attention to date. The present study aimed to evaluate the impacts of the pharmaceutical drug Carbamazepine and pH 7.1, acting alone and in combination, on the clamScrobicularia plana. For this, a long-termexposure (28 days)was conducted and a set of oxidative stress markers was investigated. The results obtained showed that S. plana was able to develop mechanisms to prevent oxidative damage when under low pH for a long period, presenting higher survival when exposed to this stressor compared to CBZ or the combination of CBZ with pH 7.1. Furthermore, the toxicity of CBZ on S. plana was synergistically increased under ocean acidification conditions (CBZ + pH 7.1): specimens survival was reduced and oxidative stress was enhanced when compared to single exposures. These findings add to the growing body of evidence that ocean acidification will act to increase the toxicity of CBZ to marine organisms,which has clear implications for coastal benthic ecosystems suffering chronic pollution from pharmaceutical drugs. KW - Ocean acidification KW - Pharmaceuticals KW - Biomarkers KW - Oxidative stress KW - Clams KW - Long-term exposures PY - 2016 DO - https://doi.org/10.1016/j.scitotenv.2015.09.138 VL - 541 SP - 977 EP - 985 PB - Elsevier B.V. AN - OPUS4-38502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pires, A. A1 - Almeida, Ângela A1 - Calisto, V. A1 - Schneider, Rudolf A1 - Esteves, V. I. A1 - Wrona, F. J. A1 - Soares, A. M. V. M. A1 - Figueira, E. A1 - Freitas, R. T1 - Long-term exposure of polychaetes to caffeine: Biochemical alterations induced in Diopatra neapolitana and Arenicola marina N2 - In the last decade studies have reported the presence of several pharmaceutical drugs in aquatic environments worldwide and an increasing effort has been done to understand the impacts induced on wildlife. Among the most abundant drugs in the environment is caffeine, which has been reported as an effective chemical anthropogenic marker. However, as for the majority of pharmaceuticals, scarce information is available on the adverse effects of caffeine on marine benthic organisms, namely polychaetes which are the most abundant group of organisms in several aquatic ecossystems. Thus, the present study aimed to evaluate the biochemical alterations induced by environmentally relevant concentrations of caffeine on the polychaete species Diopatra neapolitana and Arenicola marina. The results obtained demonstrated that after 28 days exposure oxidative stress was induced in both species, especially noticed in A. marina, resulting from the incapacity of antioxidant and biotransformation enzymes to prevent cells from lipid peroxidation. The present study further revealed that D. neapolitana used glycogen and proteins as energy to develop defense mechanisms while in A. marina these reserves were maintained independently on the exposure concentration, reinforcing the low capacity of this species to fight against oxidative stress. KW - Invertebrates KW - Pharmaceuticals KW - Oxidative stress biomarkers KW - Energy reserves PY - 2016 DO - https://doi.org/10.1016/j.envpol.2016.04.031 VL - 2016 IS - 214 SP - 456 EP - 463 PB - Elsevier Ltd. AN - OPUS4-38505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cruz, D. A1 - Almeida, Ângela A1 - Calisto, V. A1 - Esteves, V. I. A1 - Schneider, Rudolf A1 - Wrona, F. J. A1 - Soares, A. M. V. M. A1 - Figueira, E. A1 - Freitas, R. T1 - Caffeine impacts in the clam Ruditapes philippinarum: Alterations on energy reserves, metabolic activity and oxidative stress biomarkers N2 - Caffeine is known to be one of the most consumed psychoactive drugs. For this reason, caffeine is continuously released into the environment with potential impacts on inhabiting organisms. The current study evaluated the biochemical alterations induced in the clam species Ruditapes philippinarum after exposure for 28 days to caffeine (0.5, 3.0 and 18.0 mg/L). The results obtained showed that, with the increasing caffeine concentrations, an increase in clams defense mechanisms (such as antioxidant and biotransformation enzymes activity) was induced which was accompanied by an increase in protein content. Nevertheless, although an increase on defense mechanisms was observed, clams were not able to prevent cells from lipid peroxidation that increased with the increase of caffeine concentration. Furthermore, with the increase of exposure concentrations, clams increased their metabolic activity (measured by electron transport activity), reducing their energy reserves (glycogen content), to fight against oxidative stress. Overall, the present study demonstrated that caffeine may impact bivalves, even at environmentally relevant concentrations, inducing oxidative stress in organisms. The present study is an important contribution to address knowledge gaps regarding the impacts of long-term exposures to pharmaceuticals since most of the studies assessed the effects after acute exposures, most of them up to 96 h. KW - Bivalves KW - Oxidative stress KW - Pharmaceuticals KW - Long-term exposure KW - Environmentally relevant concentrations PY - 2016 DO - https://doi.org/10.1016/j.chemosphere.2016.06.068 VL - 2016 IS - 160 SP - 95 EP - 103 PB - Elsevier Ltd. AN - OPUS4-38508 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pires, A. A1 - Almeida, Ângela A1 - Calisto, V. A1 - Schneider, Rudolf A1 - Esteves, V. I. A1 - Wrona, F. J. A1 - Soares, A. M. V. M. A1 - Figueira, E. A1 - Freitas, R. T1 - Hediste diversicolor as bioindicator of pharmaceutical pollution: Results from single and combined exposure to carbamazepine and caffeine N2 - Several environmental stressors have been identified as key and/or emerging drivers of habitat change that could significantly influence marine near-shore ecosystems. These include increasing discharges of pharmaceutical contaminants into the aquatic coastal systems. Pharmaceutical drugs are often detected in aquatic environments but still information on their toxicity impacts on inhabiting species is scarce, especially when acting in combination. Furthermore, almost no information is available on the impacts of pharmaceuticals in polychaetes, often the most abundant taxon in benthic communities and commonly used as indicator species of environmental conditions. Therefore, the present study aimed to evaluate the biochemical alterations induced in the polychaete Hediste diversicolor, from a low contaminated area at the Ria de Aveiro lagoon (Portugal), by the antiepileptic drug carbamazepine (0.0 - control, 0.3, 3.0, 6.0 and 9.0 μg/L) and the stimulant caffeine (0.0 - control, 0.5, 3.0, and 18.0 μg/L), acting alone and in combination (0.3 CBZ + 0.5 CAF and 6.0 CBZ + 3.0 CAF). Glutathione Stransferases (GSTs), superoxide dismutase (SOD) and catalase (CAT) activities was determined in Hediste diversicolor from each condition. Lipid peroxidation (LPO), glutathione reduced and oxidized (GSH and GSSG), glycogen and electron transport system (ETS) were also measured. The results obtained clearly revealed that both drugs induced oxidative stress in H. diversicolor, shown by the increase on LPO levels and decrease on total glutathione and GSH/GSSG ratio with the increase of exposure concentrations. Furthermore, the present findings demonstrated that polychaetes biotransformation capacity as well as antioxidant defense mechanisms were not sufficiently efficient to fight against the excess of reactive oxygen species (ROS) leading to LPO when organisms were exposed to both drugs. Our results also demonstrated that polychaetes tended to decrease the activity of ETSwhen exposed to drugs, avoiding energy expenditurewhich may prevent them fromgreater damages. The present study further revealed that the impacts induced by the combination of both drugswere similar to those obtained at the highest drugs concentrations acting alone. KW - Invertebrates KW - Pharmaceuticals KW - Oxidative stress biomarkers KW - Energy reserves PY - 2016 DO - https://doi.org/10.1016/j.cbpc.2016.06.003 VL - 2016 IS - 188 SP - 30 EP - 38 PB - Elsevier Inc. AN - OPUS4-38509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schneider, Rudolf A1 - Oliveira, P. A1 - Almeida, Ângela A1 - Calisto, V. A1 - Esteves, V. I. A1 - Wrona, F. J. A1 - Soares, A. M. V. M. A1 - Figueira, E. A1 - Freitas, R. T1 - Physiological and biochemical alterations induced in the mussel Mytilus galloprovincialis after short and long-term exposure to carbamazepine N2 - The bivalve Mytilus galloprovincialis collected in the Ria de Aveiro, was selected to evaluate the acute and chronic effects of carbamazepine (CBZ) at environmentally relevant concentrations. CBZ is an antiepileptic drug widely found in the aquatic environment with toxic effects to inhabiting organisms. However, few studies evaluated the acute and chronic toxicity of this drug. The experiment was performed 'by exposing mussels to 0.0, 0.3, 3.0, 6.0 and 9.0 CBZ mu g/L, for 96 h and 28 days. To assess the toxicity of the drug, a battery of biomarkers related to mussels general physiological health status and oxidative stress was applied. CBZ was quantified in mussel tissues by an Enzyme-Linked Immunosorbent Assay (ELISA). The results obtained show that CBZ did not induce oxidative stress. However, our findings,demonstrated that the drug was taken up by mussels even though presenting low bioconcentration factor (BCF) values (up to 2.2). Furthermore, our results demonstrated that after a chronic exposure the physiological parameters, namely the condition and gonadosomatic indices, were negatively affected which may impair organisms' reproductive capacity with consequences to population sustainability. KW - Pharmaceuticals KW - Bivalves KW - Oxidative Stress PY - 2017 DO - https://doi.org/10.1016/j.watres.2017.03.052 SN - 0043-1354 VL - 117 SP - 102 EP - 114 PB - Elsevier Ltd. AN - OPUS4-43304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schneider, Rudolf A1 - Almeida, Ângela A1 - Calisto, V. A1 - Esteves, V. I. A1 - Soares, A. M. V. M. A1 - Figueira, E. A1 - Freitas, R. T1 - Ecotoxicity of the antihistaminic drug cetirizine to Ruditapes philippinarum clams N2 - Cetirizine (CTZ) is an antihistaminic drug present in the aquatic environment, with limited information on its toxicity to organisms inhabiting this system. This study intended to evaluate the effects of CTZ on oxidative stress and energy metabolism biomarkers in the edible clam Ruditapes philippinarum after a 28 days exposure to environmentally relevant CTZ concentrations (0.0, 0.3, 3.0, 6.0 and 12.0 mu g/L). The results obtained showed that CTZ was accumulated by clams reaching maximum concentrations (up to similar to 22 ng/g FW) at the highest CTZ exposure concentrations (6.0 and 12.0 mu g/L). The bioconcentration factor (average maximum values of similar to 5) decreased at 12.0 mu g/L reflecting a reduction in clams uptake or increase of excretion capacity at this condition. The present study revealed that, in general, clams decreased the metabolic potential after exposure to CTZ (decrease in electron transport system activity), a response that led to the maintenance of glycogen content in organisms exposed to CTZ in comparison to control values. Our findings also showed that, CTZ did not exert significant levels of oxidative injury to clams. However, comparing the control with the highest exposure concentrations (6.0 and 12.0 mu g/L) a significant increase of the antioxidant enzyme superoxide activity (similar to 53 and similar to 44%) was observed in clams exposed to CTZ. Moreover, a tendency to increase lipid peroxidation (similar to 14 and similar to 9%) and carbonyl groups on proteins (similar to 11 and similar to 3%) was observed in clams exposed to CTZ (6.0 and 12.0 mu g/L) compared to control condition. Overall the present study suggests that toxic impacts may be induced in R. philippinarum if exposed for longer periods or higher CTZ concentrations. KW - Antihistamines KW - Clams KW - Biomarkers PY - 2017 DO - https://doi.org/10.1016/j.scitotenv.2017.05.149 SN - 0048-9697 VL - 601 SP - 793 EP - 801 PB - Elsevier B.V. AN - OPUS4-43311 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -