Pesticide Residue Analysis in Food: Advances, Challenges, and Case Studies

Pesticide residue analysis in food remains a vital component of food safety and human exposure assessment, particularly as the field of exposomics encourages a more holistic view of chemical exposure across environmental and dietary sources. Analytical scientists face the dual challenge of expanding chemical coverage while maintaining the analytical rigor required for regulatory compliance and public health assessment. Recent studies demonstrate how the discipline is evolving through innovations in high-throughput mass spectrometry, improved sample preparation, and broader screening strategies. Four recent investigations—each addressing distinct analytical and matrix challenges—highlight both the progress and the remaining technical gaps in the field.

From the Exposome to Analytical Strategy

Maykel Hernández-Mesa and Ana M. García-Campaña from the University of Granada and Gaud Dervilly and Bruno Le Bizec from LABERCA propose that analytical chemistry for food contaminants must adapt to the principles of exposomics (1). Food represents a major pathway of external chemical exposure, and the exposome framework demands analytical methods that are comprehensive, flexible, and capable of detecting a wider array of known and unknown compounds. The authors emphasize the development of “mega-methods” that encompass both liquid chromatography (LC)- and gas chromatography (GC)-amenable analytes, often through harmonized workflows that build on QuEChERS and QuEChERSER sample preparation approaches.

They also highlight the growing adoption of ion mobility spectrometry (IMS) coupled to LC–high-resolution mass spectrometry (HRMS) and GC–HRMS platforms, which enhances selectivity and helps resolve isomeric and isobaric interferences. Another emerging trend is the integration of suspect screening and non-targeted analysis to capture unexpected residues or metabolites that may not be included in traditional monitoring lists. However, these advances bring new challenges, including matrix-dependent variability, data harmonization, and the need for standardized workflows across laboratories. The authors note that without harmonization in calibration, identification criteria, and data interpretation, comparability between exposomic data sets remains limited.

Simultaneous Screening of Pesticides in Date Fruits

An example of practical innovation within this broader framework is presented in a study published in Scientific Reports on a multiresidue analysis of 211 pesticides in 90 samples of date fruit, applying a QuEChERS extraction followed by parallel analysis using ultrahigh-pressure liquid chromatography (UHPLC)–MS/MS and GC–MS/MS (2). This approach ensures comprehensive coverage across the polarity and volatility spectrum of the target analytes. Reported recoveries for most compounds ranged between 77% and 119%, demonstrating good method robustness.

In addition to analytical performance, the study connects its findings to consumer safety by calculating hazard quotients, hazard indices (HI), and carcinogenic risk using Monte Carlo simulations. The authors concluded that the detected residue levels in the sampled dates pose no significant dietary risk (hazard quotient and index values below one), with the study exemplifying how analytical data can be connected to probabilistic risk assessment models.

The team concluded that their method meets the requirements for high-throughput detection of pesticide residues in date fruits and can serve as a benchmark for evaluating pesticide residues in other date fruit varieties. Translating the method to other fruit matrices with different sugar, moisture, or fiber content could require re-optimization of extraction and cleanup conditions.

UHPLC–MS/MS-Based Dietary Risk Assessment of Lufenuron

A case study published in the journal Ecotoxicology and Environmental Safety has focused on the quantification and exposure assessment of a single pesticide in a specific vegetable matrix (3). Using a validated UHPLC–MS/MS method, the authors measured lufenuron residues in Chinese cabbage samples and linked these findings to dietary exposure models for different consumer groups. Lufenuron, a benzoylurea chitin synthesis inhibitor, poses potential risks to human and ecological health. The dietary exposure assessment showed notably higher risks in rural areas (0.177–0.381%) than in urban areas (0.221–0.500%), with rural females aged 4–6 years exhibiting the peak chronic risk quotient (0.500%), surpassing all other demographic groups tracked. The researchers expressed the hope that the focus of future research should be concentrated on the dietary health of children, the age group in the highest risk category. The growing diversity of dietary habits heightens long-term dietary risks, making it increasingly important to highlight potential hazards as agricultural chemical use expands.

GC-Amenable Pesticides in Animal-Derived Foods

Extending the analytical challenge to more complex matrices, a study by the European Union Reference Laboratory for Pesticides in Food of Animal Origin and Commodities with High Fat Content (EURL-AO) in Freiburg, Germany, focused on high-fat, protein-rich samples where extraction and cleanup are notoriously difficult. The authors developed a workflow designed to isolate GC-amenable pesticides from animal food matrices while minimizing matrix suppression effects (4). The method achieved up to 85% validation rates for analytes across the various matrices and expanded analyte coverage by 40% (from 109 to 150 validated pesticides out of 196), compared with existing techniques.

Animal-derived matrices remain among the most challenging for pesticide residue analysis due to their lipid content and strong matrix interferences. The workflow enabled continuous, around-the-clock operation with reduced solvent use and optimized fat extraction, resulting in cleaner extracts, higher sample throughput, and improved quantification even in high-fat or difficult matrices like offal and fish.

Integrating Insights Across Studies

Taken together, these four studies offer a snapshot of current pesticide residue analysis, characterized by simultaneous expansion of analytical scope and refinement of matrix-specific methodologies. Several overarching themes emerge.

First, analysts must balance breadth and depth. Multi-residue workflows offer broad chemical coverage but introduce complexity and the potential for variable recoveries. Targeted single-compound methods achieve higher sensitivity but limited chemical scope. An optimal strategy may combine both: broad screening for surveillance, followed by focused quantification for risk assessment.

Second, matrix complexity continues to dictate analytical strategy. The contrast between fruit, leafy vegetable, and animal-derived samples underscores the necessity of tailoring sample preparation to each matrix.

Third, the integration of residue detection and risk assessment is now considered standard practice. Both the date fruit and lufenuron studies incorporate exposure modeling and health risk metrics, emphasizing the expectation that analytical results should directly inform safety evaluations. This trend calls for improved quantification of measurement uncertainty, matrix effects, and detection limits, since these parameters influence regulatory conclusions.

Fourth, there is a clear movement toward the integration of exposomic principles into pesticide analysis. The exposome framework encourages broader chemical coverage, non-target screening, and retrospective data mining, facilitated by high-resolution mass spectrometry and orthogonal separation techniques such as ion mobility. Yet implementing exposomic workflows requires robust databases, harmonized acquisition parameters, and standardized reporting to ensure interlaboratory comparability.

Finally, shared calibration protocols and open data exchange will be essential for building reliable exposure databases. Participation in interlaboratory studies and the use of common identification criteria can enhance reproducibility and confidence in multi-residue findings.

The evolution of pesticide residue analysis reflects both technological progress and the growing expectation that analytical chemistry contributes directly to public health understanding. The field is moving beyond simple quantification toward a systems-level view of chemical exposure. While methodological challenges remain, the discipline is aligning with the broader vision of exposomics, where chemical analysis serves as the foundation for understanding the totality of human environmental exposure. The path forward involves both technological innovation and coordinated effort to translate laboratory precision into meaningful insights for food safety and public health.

References

(1) Hernández-Mesa, M.; Dervilly, G.; Le Bizec, B.; García-Campaña, A. M. Emerging Trends and Challenges in Detecting Residues and Contaminants in Food in the Exposome Era. Advances in (U)HPLC, 2025, 22–26. 

(2) Basij, M.; Tezerji, N. S.; Shirani, M.; Mahdavi. V. Simultaneous Screening of 211 Pesticide Residues in Date Fruits in Iran and Health Risk Assessments Based on Mont Carlo Simulation. Sci. Rep. 2025, 15 (1), 6545. DOI: 10.1038/s41598-025-87638-9

(3) Fan, Z.; Liu, F.; Ren, X.; et al. Large-Scale Fate Tendency of Lufenuron During Cabbage Cultivation: New Insights into Dietary Risk and Models Comparison. Ecotoxicol. Environ. Saf. 2025, 303, 118824. DOI: 10.1016/j.ecoenv.2025.118824

(4) Buettner, A.; Polley, J.; Hardebusch, B.; Speer, K. Automation of a Modular Method (EN 1528) for Analysis of GC-amenable Pesticides in Food of Animal Origin. J. Chromatogr. A 2025, 1741, 465620. DOI: 10.1016/j.chroma.2024.465620