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Environmental fate & pathways

Monitoring data

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monitoring data
Type of information:
experimental study
Adequacy of study:
supporting study
4 (not assignable)
Rationale for reliability incl. deficiencies:
documentation insufficient for assessment

Data source

Reference Type:
Screening of Lake Sediments for Emerging Contaminants by Liquid Chromatography Atmospheric Pressure Photoionization and Electrospray Ionization Coupled to High Resolution Mass Spectrometry
Aurea C. Chiaia-Hernandez, Martin Krauss, Juliane Hollender
Bibliographic source:
Environ. Sci. Technol., 47, 976−986

Materials and methods

Principles of method if other than guideline:
Sediment extraction
Previously frozen, individual sediment layers were freeze-dried, homogenized, weighed, and transferred to stainless steel cells prepared with a 27 mm glass fiber filter and a 16.2 mm cellulose filter. Each extraction cell was loaded with 4-6 g of sediment. To increase solvent channeling 250 mg of diatomaceous earth was also added to each cell. The cells were then extracted by pressurized liquid extraction (PLE) using an ASE 350 system (Dionex, Sunnyvale, U.S.A.) at 80 °C using a mixture of the two polar aprotic solvents ethyl acetate and acetone with intermediate dielectric constants and polarity at a ratio of 70:30 (% v/v). Approximately 23 mL of each extract was spiked with 60 μL of 2.5 ng/μL internal standard mixture with an absolute amount of 150 ng of each compound. Then the extracts were evaporated using an automated evaporator system to 100 μL at 30°C. Afterwards the extracts were diluted to 2.5 mL with HPLC water.

The removal of matrix from the sediment extracts was based on a modification of the multiresidue method “QuEChERS” (Anastassiades et al., 2003). Five milliliter of acetonitrile was added to the extracts, followed by 1.6 g of MgSO4 and 0.4 g NH4Cl. The mixture was vortexed and centrifuged for 10 min at 3500 rpm. After separation, the acetonitrile phase was transferred to a graduated centrifuge tube, evaporated to 50 μL, and brought to a volume of 500 μL by adding methanol. The final extract was filtered into 2 mL autosample vials using 0.2 μm PTFE filters.
GLP compliance:
Type of measurement:
other: Occurence

Test material

Specific details on test material used for the study:
The following UV-light stabilizer (UV-LS) were investigated:


Study design

Details on sampling:
During the summer of 2010 two sediment cores were taken from the deepest part of Lake Greifensee (Switzerland). One sediment core was used for target and suspect screening of organic contaminants and was analyzed in great detail, while the other was used for confirmation. Core samples were taken with a free fall gravity corer and stored vertically in the dark at 4 °C. Individual cores were sliced into approximately 2 cm thick pieces, transferred to glass jars, closed airtight, and stored in the dark at −20 °C.

Results and discussion

Details on results:
Eventhough, Benzotriazole have a low log Kow (1.42 ± 0.64) these compounds were found at the top 8 cm of the sediment (˞20 years) with maximum concentrations of 1.4 ng/g dw during the target screening. The six investigated UV-LS were not found during the suspect screening.

Applicant's summary and conclusion

Six benzotriazole were investigated using a newly developed multiresidue method. The method was applied on sediment cores from Lake Greifensee. Non of the six invetsigated Benzotriazole were found during the suspect screening.
Executive summary:

A multiresidue method the target and suspect screening of more than 180 pharmaceuticals, personal care products, pesticides, biocides, additives, corosion inhibitors, musk fragrances, UV light stabilizers, and industrial chemicals in sediments was developed. Sediment samples were freeze-dried, extracted by pressurized liquid extraction, and cleaned up by liquid−liquid partitioning. The quantification and identification of target compounds with a broad range of physicochemical properties was carried out by liquid chromatography followed by electrospray ionization (ESI) and atmospheric pressure photoionization (APPI) coupled to high resolution Orbitrap mass spectrometry (HRMS/MS). The recoveries and precision ranged from 97-123% and 5-20%, respectively. The method detection limits range from 0.09 to 3.5 ng/gdw, while limits of quantification range from 0.29 to 12 ng/gdw. The method was applied on sediment cores from Lake Greifensee (Switzerland). Non of the six invetsigated Benzotriazole were found during the suspect screening.

The results show that biocides, musk fragrances, and other personal care products were the most frequently detected compounds with concentrations ranging from pg/gdw to ng/gdw, whereas none of the targeted pharmaceuticals were found. The concentrations of many urban contaminants originating from wastewater correlate with the highest phosphorus input into the lake as a proxy for treatment efficiency. HRMS enabled a retrospective analysis of the full-scan data acquisition allowing the detection of suspected compounds like quaternary ammonium surfactants, the biocide triclocarban, and the tentative identification of further compounds without reference standards, among others transformation products of triclosan and triclocarban.