A Validated Method for the Analysis of 142 Pesticide Residues Using Atmospheric Pressure GC Coupled with Tandem Quadrupole Mass Spectrometry

Significance of the Topic

The accurate and sensitive determination of pesticide residues in fruits and vegetables is essential to ensure food safety and regulatory compliance. Global agricultural practices rely on hundreds of pesticide active ingredients, and multi-residue methods capable of screening a broad range of chemistries at trace levels help protect consumer health and streamline laboratory workflows.

Objectives and Study Overview

This work describes the development and validation of a comprehensive method to quantify 142 GC-amenable pesticide residues in various fruit and vegetable matrices. The study aimed to achieve high sensitivity, robust selectivity, and regulatory compliance within a single atmospheric pressure gas chromatography-tandem quadrupole mass spectrometry (APGC-MS/MS) platform.

Methodology and Used Instrumentation

• Sample Preparation: QuEChERS extraction and cleanup (AOAC method) on orange, tomato, carrot and additional matrices (apple, lettuce, courgette).
• Instrumentation: Waters 7890A GC with DB-5MS column (30 m×0.25 mm×0.25 µm) and Xevo TQ-S triple quadrupole MS equipped with interchangeable APGC source.
• GC Conditions: He carrier gas at 2 mL/min; temperature program from 70 °C (1 min) to 150 °C at 15 °C/min then to 300 °C at 10 °C/min; 30 min run time; pulsed splitless injection (1 µL) with N2 makeup gas.
• MS Conditions: AP+ mode, corona 1.8 µA, cone gas 170 L/hr, auxiliary gas 250 L/hr, source temp 150 °C; water vapor introduced to enhance protonation.
• Quantification: Eight-point matrix-matched calibration (1–1000 µg/kg); data processing with TargetLynx Application Manager.

Main Results and Discussion

MRM transitions were optimized for each analyte, exploiting the softer APGC ionization to preserve protonated molecules. Linearity exceeded R2 > 0.99 across 0.1–100 ng/mL. Limits of detection ranged mostly from 0.01 to 1 µg/kg. The method exhibited excellent selectivity with no significant interferences and consistent ion ratios (RSD < 10%), meeting EU SANCO criteria. Application to real samples detected 43 pesticides, all below EU maximum residue limits.

Benefits and Practical Applications

• Simultaneous analysis of 142 pesticides in a single injection.
• Enhanced sensitivity from APGC allows tenfold dilution of extracts, reducing matrix effects and maintenance.
• Unified platform for LC- and GC-amenable compounds streamlines laboratory operations.
• Automated data processing accelerates routine quantification and quality control.

Future Trends and Opportunities

Advancements may include integration of high-resolution mass spectrometry to further improve identification confidence, expansion of compound scope beyond 200 analytes, development of greener extraction workflows, and application of machine learning for automated data interpretation and anomaly detection.

Conclusion

The validated QuEChERS–APGC-MS/MS method on a Xevo TQ-S system delivers sensitive, selective, and robust quantification of 142 pesticide residues across diverse produce matrices. It meets stringent regulatory requirements, simplifies laboratory workflows, and supports effective food safety monitoring.

References

1. Portolés T, Cherta L, Beltran J, Gledhill A, Hernández F. Enhancing MRM Experiments in GC/MS/MS Using APGC. Waters Application Note No. 720004772en, 2013.
2. Cherta L, Portolés T, Beltran J, Pitarch E, Mol JGJ, Hernández F. Application of GC-MS/MS with Atmospheric Pressure Chemical Ionization for Multi-Class Pesticides in Fruit and Vegetables. J Chrom A. 1314:224–240, 2013.