Analysis of Dioxins in Foods and Feeds Using GC-MS/MS with BEIS

Significance of the Topic

Dioxins are highly toxic persistent organic pollutants found in food and feed even at trace levels. Accurate low-level quantification is essential for food safety and regulatory compliance. Recent advances in triple quadrupole GC-MS with Boosted Efficiency Ion Source (BEIS) promise improved sensitivity and cost-effectiveness compared to high-resolution magnetic sector GC-MS.

Objectives and Overview of the Study

This study evaluated a GC-MS/MS method using BEIS to quantify polychlorinated dibenzo-p-dioxins and dibenzofurans in approximately 250 samples across 40 food and feed matrices. Key goals included benchmarking sensitivity, accuracy, and instrument durability against established GC-HRMS methods, and confirming compliance with EU regulation methods 589/2014 and 644/2017.

Methodology and Instrumentation

Sample preparation employed automated extraction (SpeedExtractor) and clean-up (GO-xHT). Final extracts were in nonane (10 µL). The GC-MS/MS system consisted of a Shimadzu GCMS-TQ 8050 with BEIS and AOC-20i/s autosampler. GC conditions used splitless injection onto a 60 m 5Sil MS column with a multi-step temperature program from 150 °C to 320 °C. MS was operated in EI mode with BEIS at 150 µA emission current; source and interface at 230 °C and 300 °C. Calibration standards ranged 0.025 to 1.0 pg/µL, following EU criteria:

• Signal-to-noise ratio ≥3:1 for the qualifier ion
• Calibration point deviation ≤30% at LOQ across the analytical series

Main Results and Discussion

Calibration achieved LOQs of 0.025 pg/µL for most congeners and 0.05 pg/µL for octa-chlorinated species, with average relative response factor deviations below 28% and high S/N ratios (≥254). Chromatograms of standards and real samples showed distinct peaks near LOQ. Quantitation values by GC-MS/MS correlated strongly with GC-HRMS at ≥1 ng/kg TEQ, with most ratios between 50% and 200%. At concentrations below 0.1 ng/kg TEQ, greater variation was observed but remained acceptable for regulatory purposes. In durability testing, over 500 alternating analyses of standards and samples showed no sensitivity loss; repeatability remained below 20% RSD.

Benefits and Practical Applications of the Method

This GC-MS/MS BEIS approach offers sensitivity comparable to GC-HRMS at lower cost and higher throughput. Automated sample prep and robust instrument performance make it suitable for routine monitoring of dioxins in diverse food and feed matrices, ensuring regulatory compliance.

Future Trends and Potential Applications

Future developments may include expansion to other persistent organic pollutants, integration with high-throughput laboratories, further optimization of ion sources for even greater sensitivity, and application of advanced data analytics and AI for faster data processing. Broader regulatory adoption is anticipated as confidence in GC-MS/MS performance grows.

Conclusion

GC-MS/MS with BEIS provides a reliable, sensitive, and durable method for dioxin analysis in food and feed, matching high-resolution methods while improving cost and throughput. It meets EU regulatory requirements and is well-suited for routine laboratory implementation.

References

• Commission Regulation (EU) 589/2014 methods for dioxins in foods
• Commission Regulation (EU) 644/2017 methods for dioxins in feeds
• Shimadzu EU Regulation Compliant GC-MS/MS Method Package for Dioxins