Quantification of polyethylene terephthalate micro- and nanoplastics in domestic wastewater using a simple three-step method.

Concerns about impact of small plastic particles, known as microplastics (<5 mm) and nanoplastics (<1 µm), together abbreviated as MNP, on the environment and on human health have increased in recent years. Polyethylene terephthalate (PET) microplastics have been detected previously in different environmental samples including freshwater and wastewater sludge. In the present study, we target all small plastic particles of PET with a diameter smaller than 5 mm ('PET MNP'). A simple three-step method of drying, (in matrix) PET depolymerization in ethylene glycol and liquid chromatography-mass spectrometry (LC-MS) analysis, was applied for the quantification of PET MNP in influents and effluents collected from ten Dutch wastewater treatment plants. The PET recovery was 98 % in the wastewater matrix. The limits of detection (LOD) for PET in influents and effluents were 2.0 µg/L and 1.2 µg/L, respectively. PET MNP was detected in all the influents (ranging from 24.9 µg/L to 680 µg/L) and most of the effluents (ranging from

Quantification of polyethylene terephthalate microplastics and nanoplastics in sands, indoor dust and sludge using a simplified in-matrix depolymerization method.

An effective 3-step method for the quantification of mass of polyethylene terephthalate microplastics and nanoplastics (PET MNPs) in complex environmental matrices was developed based on a simplified in-matrix depolymerization. Liquid chromatography (LC) coupled with ultraviolet (UV) detection was used for detection and quantification. Recoveries for PET-spiked sand samples were 99 ± 2% (1 mg/L) and 93 ± 7% (30 mg/L). The limit of quantification (LOQ) for PET was 0.4 µg/g for sand, 1 mg/g for indoor dust and 0.2 µg/g for wet sludge. This method was applied to seven beach sand samples, 20 indoor dust samples and one sewage sludge sample. PET MNPs levels in sand samples were all below the limit of detection (LOD) of LC-UV (0.1 µg/g). The concentrations of PET MNPs in indoor dust samples ranged from 1.2 to 305 mg/g and the PET MNPs in liquid sludge was 1.5 mg/L.

Analysis of recycled rubber: Development of an analytical method and determination of polycyclic aromatic hydrocarbons and heterocyclic aromatic compounds in rubber matrices.

Recycled crumb rubber (CR) is rich in compounds with unrecognized toxic potency; this study aims at the development of an analytical method that would allow identification and quantification of a very wide range of organic compounds extractable from the complex rubber matrix. The analytical set-up includes target analysis of polycyclic aromatic hydrocarbons (PAHs) and methyl-PAHs and suspect screening of raw extracts to tentatively identify primary organic compounds present, but not included in the standard target analysis of recycled rubber, followed by analytical method development and target analysis of identified compounds. Analyzed samples included weathered and new CR originating from football turf granulates, rubber mats, and end-of-life car tires (ELTs). The developed analytical method involves sonication extraction, followed by solid phase extraction (SPE) fractionation that enables simple and efficient separation of analytes with broad polarity scale. The application of SPE fractionation resolves coelution problems and simplifies the chromatograms. This analytical approach allowed to identify and quantify 46 sample specific compounds, including several heterocyclic PAHs like 2-methylthiobenzothiazole, benzonapthothiophenes, benzonaphthofuranes and aromatic amines like diphenylamine and N-phenyl-2-naphthylamine, which to our knowledge were not determined before. The PAHs concentrations determined in CR tiles purchased in Dutch and Spanish shops exceed the EU limits for articles marketed for use by the public. Furthermore, sets of methylated PAHs, dibenzothiazoles and aromatic amines were identified and quantified, and several other compounds were tentatively identified. The obtained results stress the need for expanding the list of target compounds analyzed in CR and the need for longitudinal studies on weathering processes taking place in CR.

P-gp efflux pump inhibition potential of common environmental contaminants determined in vitro.

Across different species, cellular efflux pumps such as P-glycoprotein (P-gp; also termed multidrug resistance protein 1 [MDR1]) serve as a first line of defense by transporting toxic xenobiotics out of the cell. This mechanism is also active in aquatic organisms such as mussels, fish, and their larvae. Modulation of this resistance mechanism by chemical agents occurring in the environment could result in either higher or lower internal concentrations of toxic or endogenous compounds in cells. The aim of the present study was to explore and quantify the inhibition of the P-gp efflux pumps by several ubiquitous aquatic contaminants. The calcein-acetoxymethyl ester (calcein-AM) assay commonly used in pharmacological research was established with P-gp-overexpressing Madin-Darby canine kidney cells (MDCKII-MDR1) in a 96-well plate, avoiding extra washing, centrifugation, and lysis steps. This calcein-AM-based P-gp cellular efflux pump inhibition assay (CEPIA) was used to study the inhibition by commonly occurring environmental contaminants. Among others, the compounds pentachlorophenol, perfluorooctane sulfonate, and perfluorooctanoate strongly inhibited the P-gp-mediated efflux of calcein-AM while the chloninated alkanes did not seem to interact with the transporter. The fact that common pollutants can be potent modulators of the efflux transporters is a motive to further study whether this increases the toxicity of other contaminants present in the same matrices.

Maximizing chromatographic information from environmental extracts by GCxGC-ToF-MS.

Comprehensive two-dimensional gas chromatography (GCxGC) coupled with a time-of-flight (ToF) detector allows the separation of many constituents of previously unresolved complex mixtures (UCM) of contaminants in sediment samples. In addition to the powerful chromatographic resolution, automated mass spectral deconvolution and identification system software enables a spectral deconvolution of closely eluting peaks. An extract of highly polluted sediment from the river Elbe (Czech Republic) was submitted to noninvasive extraction and fractionation, and analyzed by GCxGC-ToF-MS. More than 400 compounds were tentatively identified from three fractions. Some of the identified analytes, although not belonging to the group of priority pollutants, are known to have a toxic potential. Examples are chlorinated polycyclic aromatic hydrocarbons (PAHs), alkylated PAHs, quinones, aminoquinones, dinaphthofurans, and thiaarenes. Due to the lack of a more thorough cleanup, the life-span of the GC-column is substantially reduced, whereas the ion source of the MS needs more frequent maintenance. The procedure described is, however, not meant for routine purposes. This procedure delivers, in one run, a wealth of information that may be useful for further elucidation of toxicological properties of sediment samples by a tentative identification of previously unknown compounds.