MULTIRESIDUE PESTICIDES ANALYSIS IN FOOD MATRICES - Agilent Ultivo Triple Quadrupole LC/MS System

Importance of the Topic

Modern agriculture relies on a broad spectrum of pesticides to protect crops and ensure high yields. Regulatory bodies worldwide enforce maximum residue limits (MRLs) at low part-per-billion levels to safeguard consumer health. Achieving reliable multiresidue analysis in complex food matrices presents analytical challenges in sensitivity, selectivity, and throughput.

Study Objectives and Overview

This study demonstrates a comprehensive screening and quantitation method for 246 pesticides and metabolites in fruit, vegetable, and dried herb matrices using the Agilent Ultivo Triple Quadrupole LC/MS system. Key goals include:

• Establishing a fast, robust workflow suitable for routine food-safety laboratories.
• Validating sensitivity, accuracy, and precision at or below regulatory MRLs.
• Evaluating real-world nonorganic samples for compliance.

Methodology and Instrumentation

Sample Preparation:

• Orange and avocado (10 g) and black tea (2 g) extracted with acetonitrile and Agilent extraction salts.
• Matrix cleanup via dispersive SPE tailored for pigments, lipids, or PSA removal.

LC Conditions:

• Column: Agilent Eclipse Plus C18, 3.0 × 150 mm, 1.8 µm at 45 °C.
• Mobile phases: water and methanol with ammonium fluoride, formate, and formic acid.
• Gradient elution over 20 minutes; flow rate 0.45 mL/min; injection volume 2 µL.

MS Conditions (dMRM mode):

• Drying gas: 250 °C, 11 L/min; sheath gas: 350 °C, 12 L/min;
• Capillary ±3 500 V; nozzle ±300–1 000 V; Delta EMV ±200 V.

Used Instrumentation

• Agilent Ultivo Triple Quadrupole LC/MS with VacShield, Cyclone Ion Guide, Vortex Collision Cell, Hyperbolic Quads.
• Agilent MassHunter software for acquisition, method setup, and reporting.

Main Results and Discussion

Instrument Performance:
High-efficiency ion transmission and controlled collision-cell fragmentation produced strong signal responses for all 246 analytes spiked in black tea at 5 ng/g (figure equivalent).

Sensitivity and Precision:

• Most pesticides detected below their MRLs with 80–120 % accuracy (n ≥4/6 replicates).
• Quantitation limits: 1 ng/g in orange and avocado; 5 ng/g in black tea.
• Precision: %RSD <10 % at lowest levels for the majority of analytes.

Real-World Sample Analysis:
Nonorganic orange and avocado samples processed identically to organic matrices. Calibration curves exhibited R2 >0.99. No residues found in avocado, while three pesticides (carbaryl, propiconazole, pyrimethanil) exceeded MRLs in orange.

Practical Benefits and Applications

The Ultivo platform combines high analytical performance with a compact footprint, reducing maintenance and downtime. Its ease of use and integrated software streamline method development and reporting, making it ideal for regulatory, QA/QC, and environmental testing laboratories with varying levels of LC/MS expertise.

Future Trends and Applications

Emerging directions include:

• Integration of machine-learning algorithms in data processing for automated peak identification.
• Expansion to high-throughput, multiplexed workflows for broader pesticide panels.
• Miniaturized or ambient ionization techniques to further accelerate on-site screening.
• Linking instrument data to regulatory databases for real-time compliance monitoring.

Conclusion

This work validates the Agilent Ultivo Triple Quadrupole LC/MS as a powerful solution for routine multiresidue pesticide analysis in complex food matrices. Its robust sensitivity, precision, and streamlined workflow support reliable MRL monitoring and enhance laboratory productivity.

References

No formal literature references were provided in the original application note.