DOI: 10.3390/separations13080219 ISSN: 2297-8739

Advanced Sorbents in Miniaturized Solid-Phase Extraction for Phenolic Compounds in Plant-Derived Food Matrices: A Systematic Critical Review of Sorbent Architecture, Interaction Mechanisms, and Analytical Trends

Alejandra Caluña Padilla, Miguel A. Reinoso, Diego Barzallo

The compositional complexity of plant-derived food matrices and the structural diversity of phenolic compounds influence sample preparation, promoting miniaturized solid-phase extraction using advanced sorbents for their determination. This critical systematic review examines these sorbents over the 2016–2025 period, organizing the analysis according to their structural platform to investigate how their architecture is associated with the reported interaction mechanisms, to interpret analytical performance in the appropriate context, and to identify methodological trends, limitations, and knowledge gaps. Through a systematic search in Scopus and the application of predefined eligibility criteria, 37 studies were selected and included in the critical narrative synthesis. The analysis primarily covered molecularly imprinted sorbents, functionalized polymeric and carbon-based platforms, and layered inorganic materials. Magnetic separation using Fe3O4 emerged as the most widely employed operational strategy across the analyzed platforms, while flavonoids and phenolic acids were the predominant target subclasses. Identified gaps include the infrequent evaluation of matrix effects, the limited formal assessment of method sustainability, and the scarce experimental validation of the relative contribution of retention mechanisms in systems involving multiple simultaneous interactions. By organizing the available evidence according to sorbent structural platform, this review provides a critical framework for interpreting analytical performance, informing the rational design of advanced sorbents, and supporting the development of miniaturized solid-phase extraction techniques for food analysis.

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