Autor(es): Rede, Diana ; Vilarinho, Rui ; Delerue-Matos, Cristina ; Moreira, Joaquim Agostinho ; Fernandes, Virgínia Cruz ; Fernandes, Virgínia
Data: 2025
Identificador Persistente: http://hdl.handle.net/10400.22/29935
Origem: Repositório Científico do Instituto Politécnico do Porto
Assunto(s): Microplastics; Soil; Spectroscopic analysis; μ-Raman; Green analytical chemistry; AGREE metrics
In recent years, microplastic (MP) pollution has garnered significant attention owing to its ability to permeate various ecosystems, including soil. These particles can infiltrate the environment, either directly or through the degradation of larger plastic items. Despite growing concerns, standardized methods for quantification are still lacking. This study aimed to screen for the presence of MPs in agricultural soils while incorporating green analytical principles in the methodology. A density separation followed by centrifugation was employed, based on the principles of the QuEChERS extraction method. This approach minimized sample quantities, reagent consumption, and waste production, ensuring efficient extraction and analysis. Recovery tests using certified soils spiked with pristine MPs, specifically polystyrene, polypropylene (PP), and ethylene-vinyl acetate for larger MPs (3–5 mm), and low-density polyethylene, polyamide 6, and tire wear particles for smaller MPs (15–300 m), achieved recovery levels exceeding 69% for smaller MPs and over 91% for larger particles. Spectroscopic analysis revealed slight alterations in the Raman spectra of MPs after extraction. Transitioning to agricultural soil analysis has revealed challenges, including spectral interferences. Nine mesoplastics (5–20 mm) were detected, predominantly consisting of PP and polyethylene (PE), along with seven MPs, three of which were individually identified as PE-based, while the remainder were inconclusive, including one fiber. The evaluation of the method’s sustainability using the Analytical Eco-Scale and Analytical Greenness Calculator Metric (AGREE), with scores of 82 out of 100 and 0.66 out of 1, respectively, demonstrated its potential as a reliable approach to MP analysis in soils. This study highlights the potential of integrating green analytical chemistry principles into MP extraction methodologies and emphasizes the value of the proposed QuEChERs-based approach for improving the sustainability and efficiency of MP monitoring in agricultural soils.
