Beyond the native state: Revolutionizing food phenolic acids profiling through advanced chemical derivatization and sample pretreatment (2003-2025).

Phenolic acids, as key bioactive constituents abundantly present in plant-based foods, play a crucial role in evaluating nutritional quality, flavor characteristics, and health-promoting effects. However, their accurate analysis is severely constrained by high polarity, low volatility, structural diversity, and matrix interference inherent to complex food matrices. Chemical derivatization has emerged as an indispensable technique to overcome these challenges. Through covalent modification of reactive functional groups, properties such as volatility, thermal stability, chromatographic performance, and detection sensitivity are improved. Over the past two decades, notable innovations have been achieved, including novel derivatization reagents for GC, advanced strategies for LC-MS, and improved sample pretreatment methodologies. This review systematically consolidates progress in derivatization-based analysis of food phenolic acids since 2003. Key chromatographic platforms are critically evaluated, with emphasis on derivatization mechanisms, such as silylation, esterification, and amidation, along with their practical implementations. Sample pretreatment techniques aimed at matrix cleanup and analyte enrichment are also comprehensively examined. Furthermore, current methodological limitations are discussed, and future directions are proposed, indicating trends toward miniaturization, automation, high-throughput capacity, metabolic research, and greener analytical principles. The overarching objective is to establish a robust scientific and technical foundation for sensitive and accurate phenolic acid analysis in food science and quality control.

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