Synthesis and evaluation of a new acrylic copolymer for dispersive solid-phase microextraction of organic contaminants from urban wastewater
• Synthesis and characterization of a novel acrylic copolymer. • A Plackett-Burman design was used to evaluate extraction parameters. • A PTTANH-D-μ-SPE method was optimized to extract CECs from treated wastewater. • The method was applied to authentic wastewater effluent samples. • Scored 6/10 on the sample preparation metric of sustainability. Contaminants of emerging concern (CECs) in wastewater effluents pose significant risks to aquatic ecosystems and human health, underscoring the urgent need for effective monitoring. This study introduces a novel acrylic copolymer, Poly(TMPA-co-TEGDMA-co-AA-co-NIPAM-co-HEMA), referred to as PTTANH, functionalized with acrylic acid (AA), N-isopropyl acrylamide (NIPAM), and 2-hydroxyethyl methacrylate (2-HEMA). The copolymer was designed for dispersive solid-phase microextraction (D-μ-SPE) to extract CECs from aqueous media. The copolymer was characterized using FTIR, SEM, BET, and DSC, with key parameters optimized to develop an efficient and high degree of cross-linking and thermal stability (0–300 °C). The developed PTTANH was subsequently employed in a multi-analyte D-μ-SPE extraction method that was optimized and validated for 24 CECs from urban wastewater effluent. Samples were analyzed using LC-MS/MS. The LOD and LOQ were between 2–92 ng L −1 and 6–279 ng L −1 , respectively. The average recovery was 85 %, intra-day precision was 7 % RSD, and inter-day precision was 11 % RSD. The linear range was 100–33300 ng L −1 . The optimized protocol requires a small sample volume (12 mL), a minimal amount of sorbent (40 mg), organic solvent (4 mL), and analysis time (25 min), achieving a score of 6.0/10 on the Sample Preparation Metric of Sustainability (SPMS).
Authors
- Dimitrios Ν. Bikiaris (ORCID: https://orcid.org/0000-0001-8458-4952)
- Eirini Andreasidou (ORCID: https://orcid.org/0000-0002-9013-0081)
- Lorenzo Martello
- Ester Heath (ORCID: https://orcid.org/0000-0001-8754-6978)
- Dimitra A. Lambropoulou (ORCID: https://orcid.org/0000-0001-5743-7236)
- David Heath
Institutions
- Aristotle University of Thessaloniki (GR)
- Jožef Stefan Institute (SI)
- Jožef Stefan International Postgraduate School (SI)
- Centre for Research and Technology Hellas (GR)
Publication Details
- Journal
- Microchemical Journal
- Published
- 2025-02-13
- DOI
- https://doi.org/10.1016/j.microc.2025.113038
- Citations
- 6
- Primary Topic
- Analytical chemistry methods development
- Type
- article
- Field-Weighted Citation Impact
- 4.51
Funders
- Javna Agencija za Raziskovalno Dejavnost RS
- Horizon 2020 Framework Programme