The growing awareness of the environmental impact of analytical procedures has promoted the development of more sustainable methodologies. In this context, White Analytical Chemistry (WAC) has emerged as an approach aimed at balancing analytical performance, environmental sustainability, and operational efficiency [1]. Emerging contaminants (ECs), not yet fully regulated but under investigation due to potential environmental and health risks [2], represent a significant analytical challenge, especially at ultra-trace levels in complex matrices. This work explores a WAC-oriented strategy for determining ECs in wastewater using a biodegradable polymeric film (Mater-Bi) as extraction phase. A previously optimized method, developed through a Design of Experiments (DoE) approach, enabled the quantification of sixteen analytes - including UV filters, pharmaceuticals, and additives - achieving satisfactory recoveries, good precision, and minimal ion suppression [3]. Preliminary results also suggested the applicability of the film for perfluoroakyl substances (PFAS), although different extraction conditions were required. To better understand analyte losses, a mass balance study was conducted. Results showed weak interactions between polar compounds and the film, while PFAS were not completely desorbed during back-extraction. To address these limitations, two mixture-process designs were carried out to optimize conditioning and back-extraction phases. In the first design, three mixture variables (MeOH, EtOH, and H2O) and three process variables (extraction time, acid %, and ultrasound power) were evaluated; all were significant except ultrasound power. In the second design, six factors were investigated: three mixture variables (MeOH, EtOH, and ACN) and three process variables (number of back-extractions, extraction time, and solvent volume). All factors significantly affected the response except solvent volume, fixed at the lowest level to comply with green chemistry principles. Overall, this study demonstrates the potential of Mater-Bi as a sustainable extraction material for emerging contaminants. The mixture-process design approach improved recoveries and broadened the applicability of the biodegradable film, particularly for PFAS, supporting sustainable environmental monitoring.

A mixture-process design approach to optimize emerging contaminants extraction using a biodegradable film

Erica Ceccardi;Marina Di Carro;Emanuele Magi;Barbara Benedetti
2026-01-01

Abstract

The growing awareness of the environmental impact of analytical procedures has promoted the development of more sustainable methodologies. In this context, White Analytical Chemistry (WAC) has emerged as an approach aimed at balancing analytical performance, environmental sustainability, and operational efficiency [1]. Emerging contaminants (ECs), not yet fully regulated but under investigation due to potential environmental and health risks [2], represent a significant analytical challenge, especially at ultra-trace levels in complex matrices. This work explores a WAC-oriented strategy for determining ECs in wastewater using a biodegradable polymeric film (Mater-Bi) as extraction phase. A previously optimized method, developed through a Design of Experiments (DoE) approach, enabled the quantification of sixteen analytes - including UV filters, pharmaceuticals, and additives - achieving satisfactory recoveries, good precision, and minimal ion suppression [3]. Preliminary results also suggested the applicability of the film for perfluoroakyl substances (PFAS), although different extraction conditions were required. To better understand analyte losses, a mass balance study was conducted. Results showed weak interactions between polar compounds and the film, while PFAS were not completely desorbed during back-extraction. To address these limitations, two mixture-process designs were carried out to optimize conditioning and back-extraction phases. In the first design, three mixture variables (MeOH, EtOH, and H2O) and three process variables (extraction time, acid %, and ultrasound power) were evaluated; all were significant except ultrasound power. In the second design, six factors were investigated: three mixture variables (MeOH, EtOH, and ACN) and three process variables (number of back-extractions, extraction time, and solvent volume). All factors significantly affected the response except solvent volume, fixed at the lowest level to comply with green chemistry principles. Overall, this study demonstrates the potential of Mater-Bi as a sustainable extraction material for emerging contaminants. The mixture-process design approach improved recoveries and broadened the applicability of the biodegradable film, particularly for PFAS, supporting sustainable environmental monitoring.
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11567/1312839
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