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Targeted quantification and untargeted screening of alkylphenols, bisphenol A and phthalates in aquatic matrices using ultra-high-performance liquid chromatography coupled to hybrid Q-Orbitrap mass spectrometry
Huysman, S.; Van Meulebroek, L.; Janssens, O.; Vanryckeghem, F.; Van Langenhove, H.; Demeestere, K.; Vanhaecke, L. (2019). Targeted quantification and untargeted screening of alkylphenols, bisphenol A and phthalates in aquatic matrices using ultra-high-performance liquid chromatography coupled to hybrid Q-Orbitrap mass spectrometry. Anal. Chim. Acta 1049: 141-151. https://hdl.handle.net/10.1016/j.aca.2018.10.045
In: Analytica Chimica Acta. Elsevier: New York; Amsterdam. ISSN 0003-2670; e-ISSN 1873-4324, more
Peer reviewed article  

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Author keywords
    Phthalates; Mono-phthalates; Alkylphenols; Aquatic matrices; Orbitrap; Multi-fragmentation pathway

Authors  Top | Datasets 
  • Huysman, S., more
  • Van Meulebroek, L., more
  • Janssens, O., more
  • Vanryckeghem, F., more
  • Van Langenhove, H., more
  • Demeestere, K., more
  • Vanhaecke, L., more

Abstract
    result thereof easily released in the aquatic environment, due to different physical diffusion processes. In this context, a dedicated method was developed for the simultaneous quantification of 27 known and a virtually unlimited number of unknown alkylphenols, Bisphenol A and phthalates in 2 aquatic matrices, i.e. sea- and freshwater. To this extent, a novel instrumental HESI-UHPLC-HRMS (heated electro-spray ionization ultra-high performance liquid chromatographic high resolution mass spectrometric) method was devised for the simultaneous analysis of 7 phenols (i.e. 6 alkylphenols and Bisphenol A) and 20 phthalates within 10 min. Thereafter, a solid-phase extraction protocol was statistically (95% confidence interval, p > 0.05) optimized based on experimental designs. The method was proven fit-for-purpose through a successful validation at environmentally relevant nanomolar concentrations. Analytical precautions were taken for minimizing false-positive results to suppress in-house contamination. The method demonstrated an excellent analytical performance across all known plasticizers and plastics additives for sea- and freshwater, revealing good linearity (R2 > 0.99, n = 39), stable recoveries (98.5–105.8%), satisfactory repeatability (RSD < 8%, n = 54) and reproducibility (RSD < 10%, n = 36). Subsequently, a novel analytical strategy was devised for the tentative identification of unknown plasticizers and plastics additives using specific in-house determined fragments incorporated in a Python code. The applicability of the analytical platform was demonstrated by measuring 24 seawater samples. Interestingly, 16 out of 27 known plasticizers, plastics additives and primary metabolites could be quantified while the untargeted analysis uncovered 1042 compounds, whereof 5% (n = 46) could be assigned a plasticizer-plastics additive chemical identity, providing evidence for the severe plastic contamination status of our marine environment.

Datasets (2)
  • Advanced analysis of (emerging) organic trace contaminants in the harbours of Oostende and Zeebrugge and the Belgian coastal zone: pesticides, pharmaceuticals and personal care products, more
  • Advanced analysis of (emerging) organic trace contaminants in the harbours of Oostende and Zeebrugge and the Belgian coastal zone: steroidal EDC's, plasticizers and plastic additives, more

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