Quantitation of Over 1,000 Pesticide Residues in Tomato According to SANTE 11312/2021 Guideline

Significance of the Topic

Monitoring pesticide residues in food commodities such as tomato is critical for consumer safety, regulatory compliance, and environmental protection. With maximum residue limits (MRLs) set at low parts-per-billion levels across hundreds of compounds, analytical laboratories face challenges in sensitivity, selectivity, and throughput when screening complex food matrices.

Objectives and Study Overview

The study aimed to develop and validate a streamlined, high-throughput workflow capable of quantifying over 1,000 pesticide residues in tomato using a single QuEChERS extraction followed by complementary LC/MS/MS and GC/MS/MS analyses. Performance evaluation adhered to the European SANTE 11312/2021 guideline, assessing linearity, limit of detection, recovery, and precision.

Methodology

Tomato samples were homogenized and extracted with the Agilent Bond Elut QuEChERS EN kit. A single extract was split for parallel analysis: direct injection into LC/MS/MS and 5× dilution for GC/MS/MS. Matrix-matched calibration standards (0.5–100 µg/L) and six technical replicates at 10 µg/kg were used to assess method performance. All data acquisition employed dynamic MRM (dMRM) for optimized dwell-time distribution.

Used Instrumentation

• LC/MS/MS: Agilent 1290 Infinity II LC with 6470B triple quadrupole; ZORBAX RRHD Eclipse Plus C18 column; Jet Stream electrospray source.
• GC/MS/MS: Agilent 8890 GC with 7010C triple quadrupole; HP-5ms Ultra Inert columns in midcolumn backflush; multimode inlet; high-efficiency source.
• MassHunter optimizer and pesticide MRM databases for transition development and retention time locking.

Main Results and Discussion

Linearity: Over 98% of targets exhibited R² ≥ 0.99 across 0.5–100 µg/L. Instrument LOD: More than 97% of analytes reached LOD ≤ 10 µg/L in tomato extract; 88% met S/N ≥ 10 at 1 µg/L.

Recovery and Precision: At 10 µg/kg, 98% of compounds showed RSDr ≤ 20%, and 97% had mean recoveries within 70–120%. Matrix effects were evaluated at 10 µg/L, with matrix-matched calibration successfully compensating for any suppression or enhancement.

Complementary Techniques: LC/MS/MS covered 764 pesticides, GC/MS/MS detected 341 (including 84 overlapping compounds). Examples highlighted silafluofen’s superior sensitivity by GC/MS/MS and bifenthrin’s confirmatory dual-technique quantitation.

Benefits and Practical Applications

The combined workflow reduces sample preparation steps, accelerates turnaround time to 20 minutes per run, and lowers operating costs by using a single extraction. Retention time locking and standardized MRM databases simplify method transfer and maintenance across laboratories.

Future Trends and Applications

Advancements may include expanded databases for emerging contaminants, higher-resolution spectrometry for improved selectivity, and automated data interpretation algorithms. Integration with remote monitoring and AI-driven quality control will further enhance laboratory productivity.

Conclusion

A robust, validated workflow for quantifying over 1,000 pesticide residues in tomato according to SANTE 11312/2021 has been demonstrated. The single-extraction, dual-platform approach meets stringent regulatory criteria and offers scalable, cost-effective routine testing for food safety laboratories.

References

• SANTE 11312/2021: Analytical Quality Control and Method Validation Procedures for Pesticide Residues Analysis in Food and Feed.
• Kornas P. Quantitation of 764 Pesticide Residues in Tomato by LC/MS According to SANTE 11312/2021 Guidelines. Agilent Technologies, 5994-5847EN, 2023.
• Klink T. Quantitation of 341 Pesticide Residues in Tomato According to SANTE 11312/2021 Guideline. Agilent Technologies, 5994-6761EN, 2023.