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Peer-reviewedCC BY 4.0Analytical and Bioanalytical Chemistry

Eco-friendly method for the analysis of the soluble fraction of parabens leached from sludge of a hospital wastewater treatment plant—proof of concept

  • S. Bedoya Patiño1
  • J. P. Arrubla Vélez2
  • J. M. Grisales Bedoya2
  • M. Becerra-Herrera3
  • P. Richter4
  • E. Carasek5
  • J. J. Ríos Acevedo6
  • M. Rosero-Moreano7
7 affiliations
  1. 1Facultad de Ciencias Básicas y Tecnologías, Universidad del Quindío, 630004 Armenia, Colombia
  2. 2Facultad de Tecnología, Universidad Tecnológica de Pereira, 660003 Pereira, Colombia
  3. 3Departamento de Química, Facultad de Ciencias Experimentales, Universidad de Huelva, Huelva, Spain
  4. 4Department of Inorganic and Analytical Chemistry, Faculty of Chemical and Pharmaceutical Sciences, University of Chile, P.O. Box 233, 9170124 Santiago, Chile
  5. 5Departamento de Química, Universidad Federal de Santa Catarina, Florianópolis, 88000-000 Brasil
  6. 6Facultad de Ciencias Básicas,, Universidad Santiago de Cali, Calle 5 No 62-00, 76036 Cali, Colombia
  7. 7Grupo de Investigación en Cromatografía y Técnicas Afines GICTA, Departamento de Química, Facultad de Ciencias Exactas y Naturales, Universidad de Caldas, Calle 65 No 26-10, 170004 Manizales, Colombia
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Abstract

Developing eco-friendly analytical methods is crucial for monitoring emerging pollutants in complex matrices. This study presents a methodology based on green chemistry for determining the bioavailable fraction of methylparaben (MeP), ethylparaben (EtP), propylparaben (PrP), and butylparaben (BuP) in hospital wastewater treatment plant sludge. The approach combines in situ leaching with rotating-disk sorptive extraction (RDSE) in reverse mode, followed by direct-immersion solid-phase microextraction (DI-SPME) and headspace (HS-SPME) with on-fiber derivatization. GC-MS analysis identified the DVB/CAR/PDMS fiber as the most effective due to its high analyte affinity. Derivatization was successfully performed at room temperature in 10 min, with mass spectral match factors above 85%. The active analytical workflow (SPME extraction, on-fiber silylation, and GC-MS analysis) is completed in under 60 min per sample, enabling high-throughput screening once the parallel overnight leaching is completed. The method shows high sensitivity (LODs: 2.1–5.2 ng/g), good reproducibility (RSD < 9%), and accuracy (recoveries: 80–96% at 800 ng/g, n = 3). The four parabens were quantified in real sludge samples; MeP, EtP, and BuP were detected below their limits of quantification (< LOQ), while PrP was quantified at 20.0 ± 2.4 ng/g. Significant matrix effects (50% signal reduction) necessitated a standard additions protocol. The method’s greenness, practicality, and innovation were validated using AGREEprep (score 0.54), BAGI (score 75.0), and VIGI (score 75) metrics, confirming its high sustainability, routine feasibility, and innovative character for complex environmental sample preparation.

Graphical Abstract:

Supplementary Information: The online version contains supplementary material available at https://doi.org/10.1007/s00216-026-06762-1.

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Cite

BibTeXRIS
BibTeX
@article{patino2026ecofriendly,
  title = {{Eco-friendly method for the analysis of the soluble fraction of parabens leached from sludge of a hospital wastewater treatment plant—proof of concept}},
  author = {S. Bedoya Patiño and J. P. Arrubla Vélez and J. M. Grisales Bedoya and M. Becerra-Herrera and P. Richter and E. Carasek and J. J. Ríos Acevedo and M. Rosero-Moreano},
  journal = {Analytical and Bioanalytical Chemistry},
  year = {2026},
  month = oct,
  doi = {10.1007/s00216-026-06762-1},
  url = {https://doi.org/10.1007/s00216-026-06762-1},
  note = {CC BY 4.0},
}
RIS
TY  - JOUR
TI  - Eco-friendly method for the analysis of the soluble fraction of parabens leached from sludge of a hospital wastewater treatment plant—proof of concept
AU  - S. Bedoya Patiño
AU  - J. P. Arrubla Vélez
AU  - J. M. Grisales Bedoya
AU  - M. Becerra-Herrera
AU  - P. Richter
AU  - E. Carasek
AU  - J. J. Ríos Acevedo
AU  - M. Rosero-Moreano
PY  - 2026
DA  - 2026/10/08
JO  - Analytical and Bioanalytical Chemistry
DO  - 10.1007/s00216-026-06762-1
UR  - https://doi.org/10.1007/s00216-026-06762-1
AB  - Developing eco-friendly analytical methods is crucial for monitoring emerging pollutants in complex matrices. This study presents a methodology based on green chemistry for determining the bioavailable fraction of methylparaben (MeP), ethylparaben (EtP), propylparaben (PrP), and butylparaben (BuP) in hospital wastewater treatment plant sludge. The approach combines in situ leaching with rotating-disk sorptive extraction (RDSE) in reverse mode, followed by direct-immersion solid-phase microextraction (DI-SPME) and headspace (HS-SPME) with on-fiber derivatization. GC-MS analysis identified the DVB/CAR/PDMS fiber as the most effective due to its high analyte affinity. Derivatization was successfully performed at room temperature in 10 min, with mass spectral match factors above 85%. The active analytical workflow (SPME extraction, on-fiber silylation, and GC-MS analysis) is completed in under 60 min per sample, enabling high-throughput screening once the parallel overnight leaching is completed. The method shows high sensitivity (LODs: 2.1–5.2 ng/g), good reproducibility (RSD < 9%), and accuracy (recoveries: 80–96% at 800 ng/g, n = 3). The four parabens were quantified in real sludge samples; MeP, EtP, and BuP were detected below their limits of quantification (< LOQ), while PrP was quantified at 20.0 ± 2.4 ng/g. Significant matrix effects (50% signal reduction) necessitated a standard additions protocol. The method’s greenness, practicality, and innovation were validated using AGREEprep (score 0.54), BAGI (score 75.0), and VIGI (score 75) metrics, confirming its high sustainability, routine feasibility, and innovative character for complex environmental sample preparation.  Graphical Abstract:  Supplementary Information: The online version contains supplementary material available at https://doi.org/10.1007/s00216-026-06762-1.
SN  - 1618-2642
SN  - 1618-2650
ER  -