Multiresidue Pesticides Screening and Quantitation in Complex Food Matrices Using an Agilent Ultivo Triple Quadrupole LC/MS

Importance of the Topic

Screening and quantitation of pesticide residues in food is critical to ensure consumer safety and regulatory compliance. Maximum residue limits are often set at low part-per-billion levels in diverse and complex matrices. High-throughput, sensitive, and robust analytical methods are essential to monitor hundreds of pesticides and their metabolites simultaneously.

Objectives and Overview of the Study

This study presents a UHPLC-MS/MS multiresidue method for determining more than 250 pesticides and metabolites in complex food matrices. The method leverages the chromatographic performance of the Agilent 1290 Infinity II UHPLC system, the ionization versatility of the Jet Stream source, and the compact sensitivity of the Agilent Ultivo Triple Quadrupole LC/MS. Validation included complex matrices such as avocado, black tea, broccoli, and orange.

Methodology and Sample Preparation

Samples were extracted using a citrate-buffered QuEChERS protocol with Agilent BondElut kits. Matrix-specific dSPE cleanup steps removed pigments or lipids using primary-secondary amine, graphitized carbon, or EMR-Lipid sorbents. Citrus and vegetables were processed from 10 g of homogenate, tea from 2 g, with acetonitrile extraction and cleanup to yield clear extracts.

Used Instrumentation

• Agilent 1290 Infinity II UHPLC system: High Speed Pump, Multisampler with cooler, Multicolumn Thermostat
• Agilent Ultivo Triple Quadrupole LC/MS with Agilent Jet Stream electrospray ionization

Main Results and Discussion

Sensitivity evaluation showed most pesticides detected at 5 ng/g in tea (half of typical MRL) and at 1 ng/g (one-tenth MRL) with 80–120 accuracy. Precision studies yielded relative standard deviations below 10 percent for the majority of compounds at the lowest quantifiable level. Real-world testing of nonorganic samples revealed no residues in avocado, while three pesticides in orange and seven in broccoli exceeded MRLs. Calibration curves exhibited coefficients of determination above 0.99.

Benefits and Practical Applications

• Compact instrument footprint and simplified maintenance suitable for routine labs
• High throughput with fast polarity switching and dynamic MRM, enabling over 880 transitions per cycle
• Streamlined data acquisition and reporting via Agilent MassHunter and Quant-My-Way software for rapid sample-to-report workflows

Future Trends and Applications

Advances may include increased automation of sample preparation, integration of non-targeted screening workflows, expansion of analyte panels, real-time data analysis, and coupling with high-resolution mass spectrometry. Continued miniaturization and cloud-based data management will further enhance throughput and accessibility for QA/QC and industrial labs.

Conclusion

The Agilent Ultivo Triple Quadrupole LC/MS coupled with a 1290 Infinity II UHPLC system provides a robust, sensitive, and high-throughput solution for multiresidue pesticide analysis in complex food matrices. Its compact design, ease of use, and comprehensive workflow support make it well suited for routine food safety testing.

References

1. Regulation EC No 396/2005 of the European Parliament and of the Council of 23 February 2005 on maximum residue limits of pesticides in or on food and feed of plant and animal origin and amendments as of 18 March 2008
2. Guidance document on analytical quality control and method validation procedures for pesticides residues and analysis in food and feed, SANTE 11813/2017, 21-22 November 2017