A highly selective dispersive liquid–liquid microextraction approach based on the unique fluorous affinity for the extraction and detection of per- and polyfluoroalkyl substances coupled with high performance liquid chromatography tandem–mass spectrometry
Abstract
In the present study, a highly selective fluorous affinity-based dispersive liquid-liquid microextraction (DLLME) technique was developed for the extraction and analysis of per- and polyfluoroalkyl substances (PFASs) followed by high performance liquid chromatography tandem-mass spectrometry. Perfluoro-tert-butanol with multiple C-F bonds was chosen as the extraction solvent, which was injected into the aqueous samples with a dispersive solvent (acetonitrile) in a 120:800 (μL, v/v) mixture for PFASs enrichment. The fluorous affinity-based extraction mechanism was confirmed by the significantly higher extraction recoveries for PFASs containing multiple fluorine atoms than those for compounds with fewer or no fluorine atoms. The extraction recoveries of medium and long-chain PFASs (CF 2 > 5) exceeded 70%, except perfluoroheptanoic acid, while those of short-chain PFASs were lower than 50%, implying that the proposed DLLME may not be suitable for their extraction due to weak fluorous affinity. This highly fluoroselective DLLME technique can greatly decrease the matrix effect that occurs in mass spectrometry detection when applied to the analysis of urine samples. Under the optimum conditions, the relative recoveries of PFASs with CF 2 > 5 ranged from 80.6-121.4% for tap water, river water and urine samples spiked with concentrations of 10, 50 and 100 ng/L. The method limits of quantification for PFASs in water and urine samples were in the range of 0.6-8.7 ng/L. Furthermore, comparable concentrations of PFASs were obtained via DLLME and solid-phase extraction, confirming that the developed DLLME technique is a promising method for the extraction of PFASs in real samples.
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The hydrophobicity of extraction solvents used for DLLME tends to decrease the recovery of short-chain PFAS (17%-57% for C4-C6 PFAS).
“However, the hydrophobicity of extraction solvents used for DLLME methods tends to decrease the recovery of shortchain PFAS (17%e57% for C4eC6 PFAS).”
From Worldwide trends in tracing poly- and perfluoroalkyl substances (PFAS) in the environment (2019) · cites this paper as [38]
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- Authors
- Wang, J., Shi, Y., & Cai, Y.
- Affiliations
- Chinese Academy of Sciences (CN)
- Corresponding author
- Shi, Yali
- Venue
- Journal of Chromatography A
- Publisher
- Elsevier BV
- Published
- 2018-04
- Volume
- 1544
- Pages
- 1-7
- ISSN
- 0021-9673 (ISSN-L)
- OpenAlex
- W2790191063
- Cited by
- 64
- References
- 23
- Citations by year
- 2026: 9 · 2025: 8 · 2024: 9 · 2023: 8 · 2022: 9 · 2021: 2 · 2020: 9 · 2019: 6 · 2018: 3
- FWCI
- 3.12
- Type
- journal article
- Language
- en
- Open access
- closed
- Locations
- Journal of Chromatography A (publishedVersion)
- PubMed (publishedVersion)
- Funders
- National Natural Science Foundation of China (21537004, 21722705, 21677154, 21777182)
- Strategic Priority Research Program of the Chinese Academy of Sciences (XDB14010201)
- Topics
- Physical Sciences › Chemistry › Analytical Chemistry › Analytical chemistry methods development
- Physical Sciences › Environmental Science › Environmental Chemistry › Per- and polyfluoroalkyl substances research
- Physical Sciences › Engineering › Biomedical Engineering › Microfluidic and Capillary Electrophoresis Applications
- Keywords
- per- and polyfluoroalkyl substances, PFAS, dispersive liquid-liquid microextraction, urine samples, water samples, matrix effect reduction, short-chain PFAS, extraction recovery
- MeSH terms
- Chromatography, High Pressure Liquid, Fluorocarbons, Humans, Solvents, Mass Spectrometry, Water, Water Pollutants, Chemical, Rivers, Tandem Mass Spectrometry, Limit of Detection, Liquid Phase Microextraction
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