Analysis of 197 Pesticides in Durian by Agilent PAL 3 Autosampler and 7000E Triple Quadrupole GC/MSD

Significance of the Topic

Durian is a highly valued tropical fruit with a complex chemical composition, including high fat content, sulfur compounds, and volatiles. Accurate pesticide residue analysis in this matrix is essential for consumer safety and regulatory compliance, particularly under stringent guidelines like EU SANTE/11312/2021.

Objectives and Study Overview

The study presents a robust, sensitive method for the quantitation of 197 pesticides in durian pulp and shell. It evaluates sample extraction, cleanup, and GC-MS/MS conditions to meet recovery, precision, and sensitivity criteria required for routine high-throughput testing.

Methodology and Instrumentation

Sample Preparation
• Fresh durian pulp and shell mixed 1:1 (w/w), chopped and homogenized.
• Extraction using Agilent Bond Elut QuEChERS EN kit.
• Clean-up with Agilent Bond Elut QuEChERS Highly Pigmented dispersive SPE.
• Final extract reconstituted in acetone/hexane (1:1, v/v) and filtered (0.22 µm nylon).

Chromatography and Mass Spectrometry
• Autosampling: Agilent PAL3 with 10 µL syringe, 2 µL injection.
• GC: Agilent 8890, HP-5Q columns (2×15 m×0.25 mm, 0.25 µm), He carrier, cold splitless inlet.
• Oven program: 60 °C to 310 °C at 40 °C/min and 10 °C/min ramps.
• MS: Agilent 7000E Triple Quadrupole, dynamic MRM mode, He quench gas, N₂ collision gas.

Main Results and Discussion

• Calibration: matrix-matched from 3 to 100 ppb, R² > 0.995 for all pesticides.
• Recovery: average 80–120% at 10 ppb spike level.
• Precision: RSD < 10% for all 197 pesticides (n=10 replicates).
• Matrix effects mitigated by selecting optimized MRM transitions from the Agilent P&EP database.

Practical Benefits and Applications

• High-throughput: PAL3 autosampler accelerates sample handling and reproducibility.
• Regulatory compliance: method meets EU SANTE performance requirements.
• Versatility: applicable to complex food matrices beyond durian.

Future Trends and Potential Applications

• Expansion of compound libraries and MRM databases to cover emerging pesticides.
• Integration with automated data processing and AI for faster interpretation.
• Coupling with high-resolution MS for non-target screening.
• On-site portable GC-MS for rapid field monitoring.

Conclusion

The described workflow combining Agilent PAL3 autosampler and 7000E GC/TQ achieves reliable quantitation of 197 pesticides in durian, fulfilling rigorous accuracy and precision standards. Matrix-matched calibration and optimized MRMs ensure data quality in challenging matrices, supporting routine safety testing.

Used Instrumentation

• Agilent PAL3 Autosampler (10 µL syringe, p/n 8010-1307).
• Agilent 8890 Gas Chromatograph with HP-5Q columns (p/n 19091S-431Q).
• Agilent 7000E Triple Quadrupole GC/MSD.

References

• EU SANTE/11312/2021: Analytical quality control and method validation procedures for pesticide residues analysis in food and feed.
• Agilent MassHunter Pesticide and Environmental Pollutants MRM Database (P&EP 4.0), G9250AA.