Microextraction of Polycyclic Musks from Surface Water with Deep-Eutectic-Solvent-Coated Membrane Followed by Gas-Chromatography–Mass Spectrometry Analysis
Open accessAbstract
Deep eutectic solvents (DESs), a novel class of eco-friendly solvents, are attracting considerable attention in extraction techniques. In this study, a hydrophobic DES, created by combining a quaternary ammonium salt and hexanoic acid, was coated onto a commercial cellulose membrane for polycyclic musks (cashmeran, celestolide, galaxolide, and tonalid) microextraction from surface waters followed by gas-chromatography–mass spectrometry (GC MS) analysis. A series of DESs were synthesized and characterized to identify suitable candidates for use as a coating on cellulose membranes. A factorial design approach was employed to investigate key factors, including DES volume, membrane type, dissolving solvent volume, DES incorporation time, and extraction duration, following a preliminary selection of the DES type, membrane, and dissolving solvent. Under optimized conditions, a cellulose acetate membrane impregnated with DES (TBAB:C6, 1:3 molar ratio) was used for 1 h to extract polycyclic musks from surface water; the extract was then dissolved in methanol prior to the GC-MS analysis. The DES-coated membrane demonstrated a linear detection range from 2.5 to 100 μg/L, with limits of detection (LODs) ranging from 0.06 to 0.15 µg/L, while the LOQ values varied from 0.2 to 0.5 µg/L. The validated method was successfully applied to real samples, allowing us to find the presence of galaxolide and tonalide.
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SPE, MSPE, membrane-assisted extraction, and DES-modified sorbents are primarily designed to enhance selectivity and improve matrix purification.
“Unlike liquid-phase microextraction techniques, solid-phase extraction (SPE), magnetic solid-phase extraction (MSPE), membrane-assisted extraction, and DES-modified sorbents are primarily designed to enhance selectivity and improve matrix purification [51,72,73,76,96].”
From Eco-Friendly Deep Eutectic Solvent-Based Extraction Technologies: A Comprehensive Review of Principles, Applications, and Comparative Insights (2026) · cites this paper as [96]
Membrane-based and chromatomembrane extraction techniques generate cleaner extracts and exhibit better compatibility with continuous-flow and automated analytical platforms, as analyte transfer takes place through a precisely controlled membrane interface.
“Similarly, membrane-based and chromatomembrane extraction techniques generate cleaner extracts and exhibit better compatibility with continuous-flow and automated analytical platforms, as analyte transfer takes place through a precisely controlled membrane interface [51,73,96].”
From Eco-Friendly Deep Eutectic Solvent-Based Extraction Technologies: A Comprehensive Review of Principles, Applications, and Comparative Insights (2026) · cites this paper as [96]
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- Authors
- Terlizzi, F., Fernandes, J. O., Gonzalez, T., Petrarca, M. H., Silva, L. D. S., Lamarca, R. S., Gonzalez, M. H., Lapa, R., & Cunha, S. C.
- Affiliations
- Universidade do Porto (PT)
- LAQV-REQUIMTE, Department of Chemical Sciences, Laboratory of Bromatology and Hydrology, Faculty of Pharmacy, University of Porto, Rua Jorge Viterbo Ferreira n. º 228, 4050-313 Porto, Portugal
- Department of Chemistry and Environmental Science, National Institute for Alternative Technologies of Detection, Toxicological Evaluation and Removal of Micropollutants and Radioactives (INCT-DATREM), São Paulo State University (UNESP), São José do Rio Preto, SP 15054-000, Brazil
- Universidade Estadual Paulista (Unesp) (BR)
- Corresponding author
- Cunha, Sara C.
- ORCID
- Venue
- Chemosensors
- Publisher
- MDPI AG
- Published
- 2025-03-04
- Volume
- 13
- Issue
- 3
- Pages
- 88
- ISSN
- 2227-9040 (ISSN-L)
- OpenAlex
- W4408151905
- Cited by
- 5
- References
- 38
- Citations by year
- 2026: 4 · 2025: 1
- FWCI
- 1.89
- Type
- journal article
- Language
- en
- Open access
- gold
- doi.org
- Licence
- Locations
- Chemosensors (publishedVersion, cc-by)
- DOAJ (DOAJ: Directory of Open Access Journals) (submittedVersion, cc-by-sa)
- Funders
- PT National Funds (CleanH2O-2022.03009.PTDC)
- Topics
- Physical Sciences › Chemistry › Analytical Chemistry › Analytical chemistry methods development
- Physical Sciences › Chemical Engineering › Catalysis › Ionic liquids properties and applications
- Physical Sciences › Environmental Science › Water Science and Technology › Environmental and Analytical Chemistry Studies
- Keywords
- polycyclic musks, deep eutectic solvents, quaternary ammonium compounds, hexanoic acid, galaxolide, surface water analysis, factorial design optimization, green solvents
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