TY - JOUR A1 - Lima, D. A1 - Santos, S A1 - Scherer, H. A1 - Schneider, Rudolf A1 - Duarte, A. A1 - Santos, E. A1 - Esteves, V. T1 - Effects of organic and inorganic amendments on soil organic matter properties N2 - The aim of this work was to investigate the effects of long-term application of different organic fertilizers (sewage sludge, farmyard manure, compost) as compared to mineral fertilizer on the structure of the soil organic matter. Capillary electrophoresis was employed for the quantification of monosaccharides and phenolic compounds, whereas NMR and FT-IR were used for the overall characterization of the soils organic matter. Application of farmyard manure results in a higher content of organic matter derived from angiosperms, suggested by the higher levels of syringic and vanillic phenols. Spectroscopic studies show an increase of lignin and lignin-like products in the organic matter of the soil, which may be derived from the cereal straw supplied with farmyard manure. According to spectroscopic analysis, 13C CPMAS-NMR and FT-IR spectra, higher contents of methylene groups (– CH2) from proteins and protein-like compounds, as well as higher levels of carbohydrates, were found in the soil supplied with compost. The monosaccharide (rhamnose, xylose, glucose, mannose, arabinose, fucose and galactose) content was not significantly influenced by the different organic fertilizers, suggesting that the type of amendment used does not affect any of these six studied monomers. Comparing the three organic amendments the most significant differences were observed after long-term application of farmyard manure, with an increase in lignin and lignin-like products in the soil organic matter, and compost, which appears to contribute to an increase of protein and protein-like, as well as carbohydrates content on soil organic matter. The knowledge of such changes can be essential to understand the sorption and bioavailability of pollutants, as well as establish/unestablish ways to recycling organic residues as organic fertilizers. KW - Soil amendment KW - Organic matter charcterization KW - Phenols KW - Monosaccharide KW - CZE KW - FT-IR KW - 13C-NMR PY - 2009 DO - https://doi.org/10.1016/j.geoderma.2009.01.009 SN - 0016-7061 SN - 1872-6259 VL - 150 IS - 1-2 SP - 38 EP - 45 PB - Elsevier CY - Amsterdam AN - OPUS4-19333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liang, S. A1 - Schneider, Rudolf T1 - Capillary zone electrophoresis of cowpea mosaic virus and peak identification KW - Cowpea mosaic virus KW - CZE KW - MALDI-TOF-MS KW - Peak identification KW - Two electrophoretic forms PY - 2009 DO - https://doi.org/10.1002/elps.200800468 SN - 0173-0835 VL - 30 IS - 9 SP - 1572 EP - 1578 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-19447 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Santos, S. A1 - Costa, C. A. E. A1 - Duarte, A. C. A1 - Scherer, H. W. A1 - Schneider, Rudolf A1 - Esteves, V. I. A1 - Santos, E. B. H. T1 - Influence of different organic amendments on the potential availability of metals from soil: A study on metal fractionation and extraction kinetics by EDTA N2 - The effects of long-term application of different organic amendments, as compared to mineral fertilizer, on Zn, Cu and Pb content and leachability in a luvisol derived from loess were assessed. The organic fertilizers, applied since 1962, were compost (COM) – from green organic household waste, sewage sludge (SLU) – from municipal water treatment facilities, farmyard manure (FYM) and the doses applied since 1997 were 90 t ha-1, 10 t ha-1 and 9 t ha-1, once in 3 years, respectively. The kinetics of metals extraction with 0.05 mol dm-3 EDTA at pH 6.0 has been studied. The two first-order reactions model was fitted to the kinetic data and allowed to distinguish two pools for each metal: a 'labile' fraction (Q1), quickly extracted with a rate constant k1, and a 'moderately labile' fraction (Q2), more slowly extracted, with a rate constant k2. Simultaneously, the pseudo-total metal contents in the soil samples were determined after digestion with aqua regia (3:1 HCl + HNO3). The obtained parameters Q1, k1, Q2, k2, for the kinetics of extraction of each metal in the three replicates of each fertilization mode, as well as the pseudo-total metal contents, were statistically analysed. COM and SLU application resulted in an increase of the total contents of Pb, Zn and Cu in soil. Further, the percentage of labile Zn and Pb also increased in consequence of the application of those amendments, particularly COM. The increase was more noticeable for Zn. FYM, despite not increasing the total content of Pb, Zn or Cu, did also have an effect on the leachability of Zn and Pb, increasing their labile fraction in soil. These results point to a potential risk of increasing metals mobility in soil, mainly Zn, associated to the use of organic amendments, particularly COM or SLU. KW - Compost KW - Sewage sludge KW - Soils KW - Metal mobility KW - EDTA KW - Kinetics PY - 2010 DO - https://doi.org/10.1016/j.chemosphere.2009.11.008 SN - 0045-6535 SN - 0366-7111 VL - 78 IS - 4 SP - 389 EP - 396 PB - Elsevier Science CY - Kidlington, Oxford AN - OPUS4-22187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martínez, N.A. A1 - Schneider, Rudolf A1 - Messina, G.A. A1 - Raba, J. T1 - Modified paramagnetic beads in a microfluidic system for the determination of ethinylestradiol (EE2) in river water samples N2 - In this work, we have developed and characterized a novel microfluidic immunoassay methodology for rapid and sensitive quantification of ethinylestradiol (EE2) in river water samples. The detection of EE2 was carried out using a competitive direct immunoassay method based on the use of anti-EE2 polyclonal antibodies immobilized on magnetic microspheres 3-aminopropyl-modified manipulated for an external removable magnet. The EE2 present in the water sample was allowed to compete with EE2-horseradish peroxidase (HPR) conjugated for the immobilized anti-EE2 antibody. The HPR, in the presence of hydrogen peroxide (H2O2) catalyzes the oxidation of catechol (Q) whose back electrochemical reduction was detected on gold electrode at 0.0 V. The response current obtained from the product of enzymatic reaction is inversely proportional to the amount of EE2 in the water sample. The electrochemical detection can be done within 1 min and total assay time was 30 min. The calculated detection limits for electrochemical detection and the ELISA procedure are 0.09 and 0.32 ng L-1 respectively and the intra- and inter-assay coefficients of variation were below 5.8%. Our electrochemical immunosensor showed higher sensitivity and lower time consumed than the standard spectrophotometric detection ELISA method, which shows the potential for assessment of EE2 in river water samples. KW - Enzyme immunoassays KW - Ethinylestradiol KW - Paramagnetic beads KW - Horseradish peroxidase KW - Microfluidic KW - Flow injection analysis PY - 2010 DO - https://doi.org/10.1016/j.bios.2009.10.031 SN - 0956-5663 SN - 1873-4235 VL - 25 IS - 6 SP - 1376 EP - 1381 PB - Elsevier CY - Barking, Essex, UK AN - OPUS4-22188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lima, D.L.D. A1 - Silva, C.P. A1 - Schneider, Rudolf A1 - Esteves, V.I. T1 - Development of an ELISA procedure to study sorption of atrazine onto a sewage sludge-amended luvisol soil N2 - Pesticides may contaminate ground and surface waters and one of the major factors governing this property is soil sorption. Sorption can be assessed by batch equilibrium technique which produces lots of extracts with high dissolved organic carbon concentration in which the pesticide concentration has to be determined. We developed an ELISA procedure to analyse atrazine based on polyclonal antibodies (C193) for which tracer structure and dilutions of immunochemical reagents were adapted to fit the purpose. After a 1000-fold dilution (or after an SPE clean-up procedure) extracts of a sewage-sludge amended luvisol (used as an example application of the methodology developed) could be reliably analysed. The Freundlich model is able to describe adsorption for this system (r² = 0.977) delivering a distribution coefficient KF of 1.6 ± 0.2 (mg kg-1) (mg L-1)-N and an isotherm nonlinearity factor N of 0.70 ± 0.09. KW - ELISA KW - Atrazine KW - Sorption PY - 2011 DO - https://doi.org/10.1016/j.talanta.2011.06.024 SN - 0039-9140 VL - 85 IS - 3 SP - 1494 EP - 1499 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-24305 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Calisto, V. A1 - Bahlmann, Arnold A1 - Schneider, Rudolf A1 - Esteves, V.I. T1 - Application of an ELISA to the quantification of carbamazepine in ground, surface and wastewaters and validation with LC-MS/MS N2 - Carbamazepine is a psychiatric pharmaceutical widely detected in aquatic environments. Due to its generalized occurrence and environmental persistence it might be considered as an anthropogenic pollution indicator. In this research, a previously developed enzyme-linked immunosorbent assay (ELISA), based on a commercial monoclonal antibody, was applied to the quantification of carbamazepine in ground, surface and wastewaters and results were validated by liquid chromatography–tandem mass spectrometry (LC–MS/MS). The performance of the applied ELISA methodology was tested in the presence of high concentrations of sodium chloride and dissolved organic matter. The method was not significantly affected by matrix effects, being adequate for the quantification of carbamazepine in environmental samples, even without sample pre-treatment. This method allows the quantification of carbamazepine in the range of 0.03–10 µg L-1, with a relative error lower than 30%. Due to a pH dependent cross-reactivity with cetirizine, an antihistaminic drug, the assay also enabled the quantification of cetirizine in the samples. The application of the developed method to the quantification of carbamazepine was performed by using environmental samples with very different matrices, collected in the geographical area of Ria de Aveiro, an estuarine system located in the North of Portugal. Carbamazepine was detected in all analyzed wastewater samples and in one surface water with concentrations between 0.1 and 0.7 µg L-1. Validation with LC–MS/MS revealed that results obtained by ELISA are 2–28% overestimated, which was considered highly satisfactory due to the absence of sample pre-treatments. KW - Immunoassay KW - Pharmaceuticals KW - Environment KW - Wastewater treatment plants KW - Matrix effects KW - Cetirizine PY - 2011 DO - https://doi.org/10.1016/j.chemosphere.2011.04.072 SN - 0045-6535 SN - 0366-7111 VL - 84 IS - 11 SP - 1708 EP - 1715 PB - Elsevier Science CY - Kidlington, Oxford AN - OPUS4-24306 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Immunoanalytical Methods for the Environmental Sciences T2 - Vortrag im Rahmen des Schwerpunktes "CITE - Chemicals In The Environment" CY - Leipzig, Germany DA - 2011-12-02 PY - 2011 AN - OPUS4-24947 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Entwicklung und Validierung von Immunoassays unterschiedlicher Formate T2 - zmdb-Workshop "Trends in Bioanalysis" CY - Wildau, Germany DA - 2011-05-26 PY - 2011 AN - OPUS4-24940 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Uncertainty in Measurement with Immunoassays T2 - EURACHEM/CITAC-Workshop: Recent Development in Measurement Uncertainty CY - Lisbon, Portugal DA - 2011-06-07 PY - 2011 AN - OPUS4-24941 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Identification of unknown contaminants and metabolites of pharmaceuticals in waste water by HR-MS analysis of chromatographic fractions pre-selected by ELISA T2 - 7th Annual LC/MS/MS Workshop on Environmental Applications and Food Safety CY - Buffalo, NY, USA DA - 2011-06-13 PY - 2011 AN - OPUS4-24942 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -