Trim Time Not Columns –Multiresidue Pesticides Analysis with an Intuvo GC/TQ

Importance of the Topic

Pesticide analysis is essential to monitor residues in food and environment, ensuring compliance with stringent regulatory limits such as EU MRLs. The intensification of agriculture to meet global demand and the complexity of international food supply chains heighten the risk of banned or obsolete pesticide contamination. Robust multiresidue screening supports consumer safety and brand integrity.

Objectives and Study Overview

This work presents an integrated workflow for targeted and suspect screening of over 1100 pesticide and pollutant compounds using the Agilent Intuvo 9000 GC coupled to a 7000D Triple Quadrupole MS and optional 7250 GC/Q-TOF. The study compares targeted MRM methods for routine quantitation with high-resolution screening for unknown residues, emphasizing shortened analysis time without sacrificing performance.

Methodology and Instrumentation

Targeted analysis employed the Intuvo-7000D GC/TQ system equipped with the Agilent Pesticides & Environmental Pollutants (P&EP) MRM database containing 1161 compounds and optimized transitions. Key features include direct resistive heating, ferrule-free click-and-run connections, disposable guard chips, no-trim columns, and mid-column backflush for low carryover. Sample introduction used pulsed splitless injection with sandwich mode (matrix, sample, ISTD). Quantitative methods ran in dMRM mode with optimized dwell times and column flow under a programmed oven gradient.

The suspect screening utilized the Agilent 7250 GC/Q-TOF with an enhanced Pesticides PCDL (~1000 compounds) for high-resolution accurate mass analysis, offering three-plus orders of magnitude linear dynamic range in complex matrices.

Main Results and Discussion

Accuracy and precision were demonstrated at low ppb levels in honey, rice, and tea matrices, with most compound recoveries within 70–130% and RSDs below 15% in honey and rice. Tea showed slightly higher variability but remained within acceptable ranges. Low-level quantitation achieved EU MRL compliance at 5 ppb for key pesticides such as DDT-o,p', alachlor, and chlordane, with clear separation of MRM transitions. Robustness tests over 60 injections highlighted stable response, with minimal impact from guard chip or liner changes. The GC/Q-TOF platform delivered linearity (R2>0.999) across a 3.5-order magnitude range, facilitating suspect screening and retrospective data analysis.

Benefits and Practical Applications

• High throughput: Trimmed analysis time via direct heating and fast oven ramps reduces cycle times.
• Reduced downtime: Mid-column backflush and disposable chips lower maintenance and carryover.
• Comprehensive coverage: Extensive MRM database for targeted quantitation; high-resolution library for unknown screening.
• Regulatory compliance: Reliable quantitation at or below EU MRLs supports QA/QC and brand protection.

Future Trends and Possibilities

Integration of real-time cleaning (JetClean) and automated suspect screening workflows can further enhance lab productivity. Emerging trends include expanded high-resolution libraries, data-independent acquisition strategies, and integration with AI-driven data interpretation. Portable GC/MS systems may bring on-site multiresidue analysis and rapid decision-making to field settings.

Conclusion

The Agilent Intuvo GC/TQ and GC/Q-TOF solutions deliver rapid, sensitive, and robust platforms for both targeted and non-targeted pesticide residue analysis. Innovations in column and injector design, combined with comprehensive compound databases, enable efficient high-throughput workflows, meeting stringent regulatory demands and supporting food safety initiatives.

References

• Allington, A. Developing World Still Struggling With Obsolete Pesticides. Bloomberg BNA.
• Radio Sweden. Detection of Banned Pesticides in Produce. Sveriges Radio.
• European Crop Protection Association. Stewardship on Counterfeit and Illegal Pesticides.