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

Significance of the Topic

Rapid and reliable measurement of pesticide residues in food is essential to ensure consumer safety and regulatory compliance. With maximum residue levels set at low parts per billion, laboratories face the challenge of detecting hundreds to thousands of compounds in complex matrices. A streamlined multiresidue workflow increases throughput, reduces cost, and maintains data quality under the SANTE 11312/2021 guideline.

Objectives and Study Overview

The study aimed to develop and validate a single-sample multiresidue assay for over 1 000 pesticides in tomato. Key goals included simultaneous quantitation by liquid chromatography tandem mass spectrometry and gas chromatography tandem mass spectrometry, a 20-minute total run time per analysis, and adherence to regulatory performance requirements for sensitivity, linearity, precision and recovery.

Methodology and Instrumentation

A one-step QuEChERS extraction using a commercial Agilent Bond Elut kit provided raw extract for both techniques without further cleanup. Aliquots were split for:

• LC/MS/MS analysis on an Agilent 1290 Infinity II system coupled to a 6470B triple quadrupole operated in dynamic MRM with Jet Stream electrospray ionization
• GC/MS/MS analysis on an Agilent 8890 gas chromatograph with multimode inlet and dual mid-column backflush columns coupled to a 7010C triple quadrupole in dynamic MRM

Matrix-matched calibration standards (0.5 to 100 μg/L) and spiked quality controls (10 μg/kg) ensured accurate quantitation. Agilent pesticide MRM databases were used to define transitions, ion source voltages, and collision energies.

Main Results and Discussion

Performance met or exceeded SANTE 11312/2021 criteria:

• Linearity: Over 98% of compounds showed R2 ≥ 0.99 across eight calibration levels
• Instrument LOD: 97% of analytes at or below 10 μg/L and 88% at or below 1 μg/L
• Precision: 98% of compounds had repeatability (RSDr) ≤ 20% at 10 μg/kg
• Recovery: Mean recoveries of 70–120% for 97% of targets
• Matrix effects: Controlled via matrix-matched calibration, with signal suppression/enhancement typically < 20%

Case studies illustrated complementary strengths: silafluofen gave improved sensitivity by GC/MS/MS, while bifenthrin could be confirmed by both techniques.

Benefits and Practical Applications

The unified workflow accelerates routine pesticide testing by enabling a single extraction and two 20-minute analyses per sample. Dynamic MRM acquisition provides high sensitivity and selectivity for over 1 000 compounds, reducing instrument time and laboratory cost. The method supports compliance with European MRL regulations and can be adopted for high-throughput food safety monitoring.

Future Trends and Potential Applications

Advancements may include:

• Extension to additional food matrices such as cereals, fruits, and processed products
• Integration of high-resolution accurate-mass MS for non-target screening and metabolite identification
• Automated sample preparation robotics to further increase throughput
• Enhanced data analytics and cloud-based workflows for global method standardization
• Expansion of pesticide databases to cover emerging chemistries and transformation products

Conclusion

A robust, validated multiresidue workflow combining QuEChERS extraction with LC/MS/MS and GC/MS/MS meets stringent regulatory requirements for sensitivity, linearity, precision and recovery. It offers a cost-effective, high-throughput solution for comprehensive monitoring of over 1 000 pesticide residues in tomato.

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 application note 5994-5847EN 2023
• Klink T Quantitation of 341 Pesticide Residues in Tomato According to SANTE 11312/2021 Guideline Agilent Technologies application note 5994-6761EN 2023
• Agilent MassHunter pesticide and environmental pollutants MRM database P&EP 4.0 G9250AA