Person: Fettig, Ina
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Veröffentlichung Exploring unknown per- and polyfluoroalkyl substances in the German environment - The total oxidizable precursor assay as helpful tool in research and regulation(2021) Göckener, Bernd; Fettig, Ina; Fliedner, Annette; Rüdel, Heinz; Koschorreck, JanLimnetic, marine and soil samples of the German environmental specimen bank (ESB) were analyzed for per- and polyfluoroalkyl substances (PFAS) using target analysis and a modified total oxidizable precursor (TOP) assay (direct TOP assay (dTOP)) that works without prior extraction. Target analysis determined (Sigma)PFAS concentrations in bream livers of 8.7-282 (my)g kg-1 wet weight (ww) in 2019, with highest contaminations in the Rhine and lower Elbe. In bream fillet, concentrations were lower (<0.5-10.6 (my)g kg-1 (Sigma)PFAS). Contamination of suspended particulate matter (SPM) was highest in the upper Elbe downstream the Czech border (5.5 (my)g kg-1 dry weight (dw) in 2018). Herring gull eggs from the North and Baltic Seas showed (Sigma)PFAS levels around 53.0-69.6 (my)g kg-1 ww in 2019. In soil, concentrations ranged between <0.5 and 4.6 (my)g kg-1 dw with highest levels in the Dueben Heath near Leipzig and the low mountain range Solling. PFOS dominated in most samples. Of the targeted precursors, only FOSA, EtFOSAA, MeFOSAA, 6:2-FtS and 6:2 diPAP were found. Replacement chemicals (ADONA, HFPO-DA, F-53B) were not detected. The dTOP assay revealed that considerable amounts of precursors were present at most riverine sampling sites. Particularly high precursor concentrations were observed in samples from the Upper Elbe at the Czech border and the Upper and Middle Rhine. In herring gull eggs and most soil samples, though, concentrations of precursors were low. Time trend analysis showed decreasing trends for most detected PFAS since 2005. In SPM, however, C4-C6 perfluoroalkyl carboxylic acids seem to increase indicating growing use of precursors based on shorter fluorinated chains. The results demonstrate that target analysis detects only a minor fraction of the PFAS burdens in environmental samples. The dTOP assay can support risk assessment and chemical monitoring with more comprehensive exposure data of the actual contamination. © 2021 The Author(s).Veröffentlichung Hg isotopic composition of one-year-old spruce shoots: Application to long-term Hg atmospheric monitoring in Germany(2021) Yamakawa, Akane; Amouroux, David; Fettig, Ina; Tessier, Emmanuel; Koschorreck, JanThe Hg isotopic composition of 1-year-old Norway spruce (Picea abies) shoots collected from Saarland cornurbation Warndt, Germany, since 1985 by the German Environmental Specimen Bank, were measured for a better understanding of the temporal trends of Hg sources. The isotopic data showed that Hg was mainly taken up as gaseous element mercury (GEM) and underwent oxidation in the spruce needles; this led to a significant decrease in the δ202Hg compared with the atmospheric Hg isotopic composition observed for deciduous leaves and epiphytic lichens. Observation of the odd mass-independent isotopic fractionation (MIF) indicated that ÎÌ199Hg and ÎÌ201Hg were close to but slightly lower than the actual values recorded from the atmospheric measurement of the GEM isotopic composition in non-contaminated sites in U.S. and Europe, whereas observation of the even-MIF indicated almost no differences for ÎÌ200Hg. This confirmed that GEM is a major source of Hg accumulation in spruce shoots. Interestingly, the Hg isotopic composition in the spruce shoots did not change very significantly during the study period of >30 years, even as the Hg concentration decreased significantly. Even-MIF (ÎÌ200Hg) and mass-dependent fractionation (MDF) (δ202Hg) of the Hg isotopes exhibited slight decrease with time, whereas odd-MIF did not show any clear trend. These results suggest a close link between the long-term evolution of GEM isotopic composition in the air and the isotopic composition of bioaccumulated Hg altered by mass-dependent fraction in the spruce shoots. © 2021 The AuthorsVeröffentlichung A novel GC-MS method for the determination and quantification of metformin in surface water(2017) Goedecke, Caroline; Fettig, Ina; Piechotta, C.Drug therapy for diabetes mellitus has increased significantly in recent years. 1,1-Dimethylbiguanide hydrochloride (metformin) is the most common drug used for the treatment of diabetes. Metformin is not metabolized in the human body and enters the water cycle via sewage. A new gas chromatography-mass spectrometry (GC-MS) method has been developed which enables the quantification of metformin in surface water samples even at low concentrations in the ng L-1 range. A solid phase extraction (SPE) method for the preconcentration of metformin and the internal standard 1-butylbiguanide (buformin) was established, and the method parameters such as the composition and volume of the eluent were optimized. Derivatization of metformin and buformin was obtained by using n-methyl-bis (trifluoroacetamide) (MBTFA). The reaction conditions of the derivatization, such as the reaction temperature and volume of the derivatization agent, were evaluated. The limit of detection (LOD) and limit of quantification (LOQ) were determined to be 3.9 ng L-1 and 12 ng L-1 in surface water samples. Linearity was shown over a concentration range of 10-50 ng L-1. The good performance of the method was demonstrated by comparison with a liquid chromatography tandem mass spectrometry (LC-MS/MS) method. The results indicate that the GC-MS method is a reliable and sensitive alternative for the quantification of metformin in surface water. Quelle: http://pubs.rsc.orgVeröffentlichung Determination of tributyltin in whole water matrices under the European Water Framework Directive(2016) Richter, Janine; Fettig, Ina; Philipp, Rosemarie; Jakubowskia, Norbert; Panne, Ulrich; Fisicaro, Paola; Alasonati, EnricaMonitoring of water quality is important to control water pollution. Contamination of the aquatic system has a large effect on human health and the environment. Under the European Water Framework Directive (WFD) 2000/60/EC and the related directive on environmental quality standards (EQS) in the field of water policy 2008/105/EC, the need for sensitive reference methods was highlighted. Since tributyltin (TBT) is one of the WFD listed priority substances a method was developed which is capable to qualify and quantify the pollutant at the required low WFD EQS of 0.2 ng L-1 in whole water bodies, i.e. in non-filtered water samples with dissolved organic carbon and suspended particulate matter. Therefore special attention was paid on the interaction of TBT with the suspended particulate matter and humic substances to obtain a complete representation of the pollution in surface waters. Different water samples were investigated varying the content of organic dissolved and suspended matter. Quantification was performed using species-specific isotope dilution (SSID) and gas chromatography with inductively coupled plasma mass spectrometry (GC-ICP-MS). Different sample treatment strategies were evaluated and compared. The process of internal standard addition was investigated and optimized, hence the equilibrium between internal standards and matrix is of primary importance to perform accurate SSID. Samples spiked at EQS level were analyzed with a recovery between 95 and 105 %. Additionally real surface water samples were investigated and the TBT concentration for the whole water body was determined and compared with conventional routine analysis method.Quelle: http://www.sciencedirect.com