Quantitative Determination of Multi-Class Multi-Residue Pesticides in Edible Oil Using Captiva EMR-Lipid Cleanup by GC/MS/MS

Significance of the Topic

This study addresses the critical challenge of detecting low‐level, fat‐soluble pesticide residues in edible oils. Lipid matrices often interfere with instrument performance and quantitation accuracy. Effective lipid removal without analyte loss is essential for reliable multi‐class pesticide monitoring in food safety and regulatory compliance.

Objectives and Study Overview

The authors aimed to develop and validate a streamlined sample preparation and GC/MS/MS method using Captiva EMR-Lipid cleanup for the quantitative determination of 46 representative pesticides in olive oil, corn oil, canola oil, and soybean oil. Key goals included maximizing analyte recovery, improving cleanup efficiency, and demonstrating method performance across multiple oil matrices.

Methodology and Instrumentation

Sample Preparation Workflow:

• Accurately weigh 2.5 mL of oil and add 5 mL of 20:80 ethyl acetate/acetonitrile.
• Vortex for 15 min and centrifuge at 5000 rpm for 5 min; transfer supernatant and repeat extraction.
• Combine extracts, add water (20% final), and load onto a Captiva EMR-Lipid cartridge for gravity‐driven elution.
• Dry the eluent with MgSO₄, centrifuge, and transfer for GC/MS/MS analysis.

Instrumentation Used:

• GC: Agilent 7980B with HP-5ms Ultra Inert column (0.25 mm × 15 m, 0.25 μm).
• Carrier gas: Helium at 1.0 mL/min (column 1) and 1.2 mL/min (column 2).
• Inlet: Pulsed cold splitless (60 °C → 300 °C at 600 °C/min).
• Temperature program: 60 °C hold, ramps to 150 °C, 200 °C, then 300 °C.
• MS: Agilent 7010C Triple Quadrupole in dMRM mode; source and transfer line at 280 °C; collision gas flows optimized.

Main Results and Discussion

Calibration and Linearity:

• Regression coefficients (R²) exceeded 0.994 for representative pesticides across all oil matrices at 1–500 ng/mL.

Analyte Recovery and Precision:

• Recoveries ranged from 60 % to 120 % for over 95 % of pesticides at 10 ng/mL spiking.
• Precision (RSD) was below 20 % at low, mid, and high concentration levels (1, 10, 100 ng/mL).

Lipid Removal Efficiency:

• EMR-Lipid cleanup removed 98–99 % of co‐extractives, delivering cleaner extracts compared to QuEChERS (33–62 % removal).

Representative GC/MS/MS chromatograms demonstrated sharp peaks, minimal baseline noise, and clear separation of pesticide classes.

Benefits and Practical Applications of the Method

• Highly efficient lipid cleanup improves instrument robustness and reduces maintenance.
• Strong analyte recoveries ensure accurate quantitation for regulatory testing.
• Simplified workflow with commercially available cartridges enhances laboratory throughput.
• Validated across multiple edible oil types for broad applicability in food safety laboratories.

Future Trends and Applications

Emerging directions include integration with high‐resolution mass spectrometry for non‐target screening, automation of EMR cleanup for high‐throughput workflows, miniaturized extraction formats to reduce solvent use, and application to other complex lipid‐rich matrices such as dairy and animal tissues. Advances in sorbent materials and greener solvents will further enhance sustainability.

Conclusion

The developed GC/MS/MS method with Captiva EMR-Lipid cleanup provides a simple, robust, and reliable solution for multi‐class pesticide analysis in edible oils. Excellent linearity, accuracy, precision, and lipid removal demonstrate its suitability for routine food safety and quality control testing.

References

No independent literature references were provided in the source document.