Dioxins Analysis in Food and Feed by Intuvo 9000/7010 GC-QQQ System

Significance of the Topic

Dioxins and furans are persistent organic pollutants that bioaccumulate through the food chain and pose serious health risks. Regulatory limits demand robust analytical methods to detect trace levels of these compounds in food and feed samples.

Objectives and Study Overview

This study presents two gas chromatography–tandem quadrupole mass spectrometry methods using an Agilent Intuvo 9000/7010 system with a high-efficiency ion source. Goals include reducing analysis time, maintaining high sensitivity, and meeting regulatory requirements established by EU Commission Regulation 709/2014.

Methodology

A sample preparation workflow involving fat extraction and multicolumn cleanup was applied to fortified standards. Two separation protocols were developed:

• 52.5-minute temperature program compatible with traditional GC ovens
• 31.12-minute accelerated method exploiting Intuvo 9000’s direct column heating

Instrumentation Used

• Agilent Intuvo 9000 gas chromatograph with split/splitless inlet
• Agilent 7010 triple quadrupole mass spectrometer equipped with a high-efficiency ion source (HES)
• DB-5MS Ultra Inert capillary column (60 m × 250 µm, 0.25 µm film)

Main Results and Discussion

Both methods delivered excellent chromatographic separation for 17 target PCDD/PCDF congeners and labeled internal standards. Calibration curves exhibited coefficients of determination (R2) above 0.9997. Instrumental limits of quantitation were in the low femtogram range with signal-to-noise ratios exceeding 14. The accelerated method matched the performance of the longer run, achieving average RSD below 8% across analytes. Halving the injection volume to 0.5 µL maintained precision and sensitivity, supporting reduced sample requirements.

Benefits and Practical Applications

• Up to 40% reduction in runtime enhances sample throughput for high-volume compliance testing
• Maintained femtogram-level detection ensures conformity with EU maximum levels for dioxins and PCBs
• Smaller injection volumes reduce solvent consumption and waste generation

Future Trends and Opportunities

Advances in direct-heated GC technology and ion source design will further accelerate separations and enhance sensitivity. Integration with automated sample preparation platforms may reduce labor requirements and operational costs. Emerging high-speed mass spectrometers could enable real-time screening of persistent organic pollutants in complex matrices.

Conclusion

The Agilent Intuvo 9000/7010 GC-QQQ platform effectively identifies and quantifies trace dioxins and furans in food and feed. Both standard and accelerated methods comply with regulatory mandates, offering flexibility for diverse laboratory workflows and increased productivity without sacrificing data quality.

References

• US EPA Method 1613B: Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution HRGC/HRMS
• Commission Regulation (EU) No. 709/2014 on determination of dioxins and PCB levels in food and feed
• Riener J. Validation of a Confirmatory GC/MS/MS Method for Dioxins and Dioxin-like PCBs to Meet EU Regulation Requirements (Agilent Application Note, 2016)