Development and Validation of a Routine Multi-Residue Method for the Quantitative Determination of Pesticide Residues in Fruits, Vegetables, and Rice Using UPLC-MS/MS

Importance of the Topic

Multi-residue pesticide analysis in fruits, vegetables, and rice is essential for ensuring food safety, regulatory compliance, and facilitating global trade. The combination of simplified QuEChERS extraction with UPLC-MS/MS offers rapid, sensitive, and cost-effective monitoring of hundreds of pesticide residues.

Objectives and Study Overview

This work aimed to develop and validate a robust, quantitative method for 204 LC-amenable pesticides in commodity group 1 (high-water matrices) and group 5 (high-starch matrices) following a DisQuE QuEChERS protocol coupled to a Waters ACQUITY UPLC I-Class PLUS System with Xevo TQ-S cronos Tandem Quadrupole MS.

Methodology and Instrumentation

Samples of cucumber, tomato, red and green pepper, and brown rice were extracted using a CEN QuEChERS procedure (acidified MeCN, salting out, dispersive SPE with MgSO4 and PSA), diluted with aqueous mobile phase, and analyzed by UPLC-MS/MS. A 19 min gradient on an ACQUITY UPLC HSS T3 column (2.1 × 100 mm, 1.8 μm) at 45 °C with polarity switching enabled high-throughput data acquisition. Mass parameters (MRM transitions, cone voltage, collision energy) were sourced from the Quanpedia database and manually verified for representative compounds.

Instrumentation Used

• Waters ACQUITY UPLC I-Class PLUS System
• Xevo TQ-S cronos Tandem Quadrupole Mass Spectrometer
• MassLynx 4.2 and TargetLynx XS software
• ACQUITY UPLC HSS T3 column

Key Results and Discussion

• Linearity: R2 ≥ 0.99 over 0.001–0.1 mg/kg; residuals < 20%
• Sensitivity: LOQs ≤ 0.01 mg/kg for all targets; 93% ≤ 0.005 mg/kg
• Matrix Effects: ± 20% response deviation for > 80% of pesticides across all matrices
• Precision: inter-day RSD ≤ 20% at default MRL levels; instrument robustness RSD ≤ 3% over > 200 injections
• Specificity: no significant interferences in blanks

Benefits and Practical Applications

This validated method supports routine quality control and regulatory monitoring, offering high sensitivity, wide dynamic range, fast analysis, and reduced downtime. It enables laboratories to efficiently screen diverse commodities against EU MRLs and adapt to global trade requirements.

Future Trends and Opportunities

Advancements may include automation of sample preparation, expansion to high-resolution MS for non-target screening, integration with data analytics for trend monitoring, and extension to metabolite and degradation product analysis.

Conclusion

The DisQuE QuEChERS and UPLC-MS/MS workflow on the Xevo TQ-S cronos platform delivers a reliable, high-throughput multi-residue pesticide method, meeting stringent validation criteria and offering robust performance for routine food safety testing.

References

• Regulation (EU) 2017/660 on coordinated multiannual control program of the Union for 2018–2020
• SANTE/11813/2017: Method Validation and Quality Control Procedures for Pesticide Residues
• Waters LC Multiresidue Pesticide Standards Kit Care and Use Manual, 720005342EN
• Rapid Alert System for Food and Feed (RASFF) portal, European Commission