A critical review of LC-MS/MS based approaches for multiresidue pesticide monitoring in food commodities

Monitoring pesticide residues in food is essential for global food safety and regulatory compliance, facing increasing challenges from complex matrices, an expanding diversity of pesticide active substances, and strict maximum residue limits. This review critically examines seventy LC-MS/MS studies of pesticide residues published between 2021 and 2025, focusing on extraction and clean-up methods, analytical performance, and regulatory relevance across different food commodities. This study shows that QuEChERS-based workflows dominate current practice, constituting about three-quarters of validated methods due to their robustness, scalability, and regulatory acceptance. However, performance varies greatly depending on the matrix, with lipid, pigment, and sugar-rich commodities often needing additional clean-up or calibration techniques. A key finding is that conventional QuEChERS methods remain inadequate for highly polar pesticides such as glyphosate, aminomethylphosphonic acid (AMPA), and fosetyl-Al, which consistently exhibited reduced recoveries, higher limits of quantification, and significant matrix effects across various food commodities. Although mitigation strategies like hydrophilic interaction liquid chromatography (HILIC), ion-exchange separation, isotopic dilution, and derivatization have been explored, no universally reliable and regulatory-validated solution has been established yet. Alternative extraction strategies and green approaches demonstrate clear advantages in certain matrices, especially in reducing solvent use or improving clean-up efficiency, but are limited by reproducibility issues and a lack of inter-laboratory validation. The review also considers the impact of food processing on pesticide residue levels and analytical performance, highlighting the importance of processing-aware validation for accurate exposure assessment. Furthermore, while high-resolution mass spectrometry (HRMS) expands analytical scope for non-target screening, its routine regulatory adoption remains limited by the absence of harmonized validation criteria and data-processing challenges. The review suggests that advances in pesticide residue analysis will depend on integrating robust extraction strategies, addressing polar pesticide detection challenges, and aligning methodological innovations with regulatory validation standards to enable reliable and scalable food safety monitoring.