Determination of 208 Pesticide Residues and their Metabolites in Foods Using Oasis PRiME HLB and Xevo TQ-GC

Significance of the Topic

The accurate determination of a broad spectrum of pesticide residues and their metabolites in food commodities is essential to protect public health and ensure regulatory compliance. The use of robust sample preparation and sensitive detection techniques underpins reliable monitoring programs for fruits, vegetables, cereals, and nuts.

Study Objectives and Overview

This work presents a validated workflow for the simultaneous quantification of 208 pesticide residues and their metabolites in foodstuffs of plant origin. The method combines QuEChERS extraction with an Oasis PRiME HLB pass-through cleanup and analysis by Xevo TQ-GC triple quadrupole GC-MS/MS. Verification was conducted in accordance with the Chinese National Standard GB 23200.113-2018 and the SANTE/11813/2017 guidance document.

Methodology and Sample Preparation

• Extraction: Modified CEN 15662 QuEChERS protocol using acetonitrile for fruits, vegetables, cereals, and nuts.
• Cleanup: Pass-through solid-phase extraction with Oasis PRiME HLB cartridges, removing pigments, fats, and phospholipids efficiently without graphitized carbon black.
• Concentration and Reconstitution: Eluates evaporated to dryness, reconstituted in ethyl acetate, spiked with internal standards, filtered, and transferred to GC vials.

Used Instrumentation

• Xevo TQ-GC system operating in EI mode (70 eV), source temperature 250 °C, interface 300 °C.
• Rtx-1701 column (30 m × 0.25 mm × 0.25 µm), helium carrier (1.0 mL/min), pulsed splitless injection (1 µL).
• DisQuE QuEChERS kits, Oasis PRiME HLB Plus cartridges, TruView LCMS certified vials, MassLynx software with Quanpedia database and IntelliStart custom resolution.

Main Results and Discussion

• Cleanup Performance: Oasis PRiME HLB effectively removed pigments and co-extractives, reducing contamination of the GC inlet and extending consumable life.
• Calibration and Quantification: Matrix-matched calibration from 0.005 to 0.2 mg/kg with 1/x weighting produced back-calculated concentrations within ±20% tolerance.
• Method Performance: Over 95% of the 208 analytes met trueness criteria (70–120% recovery) and precision criteria (RSD <20%) at LOQs of 0.01–0.02 mg/kg in cucumber, grape, and rice.
• Identification Criteria: Retention time deviations were within ±0.1 min and ion ratio variations within ±30%, complying with SANTE guidelines.

Benefits and Practical Applications

• Regulatory Compliance: Fully meets GB 23200.113-2018 and SANTE/11813/2017 validation requirements.
• Workflow Efficiency: Three-click method creation via Quanpedia accelerates setup for multi-residue analyses.
• Analytical Robustness: Simplified SPE cleanup reduces development time and maintenance frequency while maintaining accuracy and sensitivity across diverse matrices.

Future Trends and Potential Directions

Future developments may include further miniaturization of SPE devices, integration of automated robotics for sample handling, expansion of spectral libraries, and application of machine-learning algorithms to improve compound identification and quantification. Harmonization of international standards will continue to streamline multi-residue pesticide testing globally.

Conclusion

The combined QuEChERS/Oasis PRiME HLB cleanup with Xevo TQ-GC analysis provides a reliable, high-throughput method for the determination of 208 pesticide residues and metabolites in plant-derived foods. It delivers excellent sensitivity, precision, and compliance with stringent regulatory criteria.

Reference

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• GB 23200.113-2018. National Food Safety Standard: Determination of 208 Pesticides and Their Metabolites in Plant-Derived Foods by GC-MS/MS.
• SANTE/11813/2017. Analytical Quality Control and Method Validation Procedures for Pesticide Residue Analysis in Food and Feed.
• CEN-EN 15662. Foods of Plant Origin – Multimethod for the Determination of Pesticide Residues.
• Waters. Oasis PRiME HLB Cartridges for Rapid and Effective Removal of Chlorophyll from QuEChERS Spinach Extracts. 2018.
• Waters. GC-MS/MS Method Development Made Easy using Xevo TQ-GC and Quanpedia Database. 2018.