DIOXIN: Routine, regulatory analysis of dioxins and dioxin-like compounds in food and feed samples

Significance of the topic

Due to their persistence and toxicity, PCDD/Fs and PCBs accumulate in fatty tissues of animals and enter the human food chain, posing significant health risks. Accurate monitoring of these persistent organic pollutants in food and feed is critical to ensure compliance with regulatory limits and to protect public health.

Objectives and Study Overview

This study aimed to validate the Thermo Scientific TSQ 9000 GC-MS/MS system with AEI source and Chromeleon CDS software for routine, regulatory-compliant analysis of PCDD/Fs, dioxin-like PCBs, and indicator PCBs in food and feed matrices. Two separate laboratories (UK and US) evaluated system performance using calibration-based LOQ determination across certified reference, proficiency test, and diverse sample types.

Methodology and Instrumentation

Samples were extracted by Twisselmann hot extraction or pressurized liquid extraction, followed by automated clean-up on a DEXTech Plus system with multilayer acidic silica, alumina, and carbon columns. Analysis employed a TRACE 1310 GC with TG-Dioxin column and a Thermo Scientific TSQ 9000 triple quadrupole MS with advanced EI source. Timed SRM acquisition used unit mass resolution, argon collision gas, and optimized GC injection protocols (large volume and splitless modes) enabled sensitive detection.

Results and Discussion

Calibration curves demonstrated linearity (R2>0.996) over four to five orders of magnitude with response factor RSDs below 6%. Calibration-based LOQs achieved upper bound WHO-PCDD/F-TEQ of 0.15 pg/g for a 2 g sample with 20 µL injection. Repeatability tests on mixed fat QC (n=14) yielded 2.7% RSD, and system robustness was confirmed over 39 injections without maintenance. Measured WHO-PCDD/F-TEQs and PCB-TEQs correlated strongly with reference data (R>0.99) across various matrices.

Benefits and Practical Applications

The validated TSQ 9000 AEI method meets EU requirements for confirmatory dioxin analysis at one-fifth of maximum levels, providing high sensitivity, precision, and uptime. Integrated Chromeleon software streamlines method setup, data processing, and compliant reporting, reducing manual steps and errors. This workflow supports high-throughput testing in regulatory, QA/QC, and research laboratories.

Future Trends and Potential Uses

Further automation of sample preparation and application of AI-driven data review may enhance throughput and interpretive accuracy. The methodology could expand to environmental monitoring, bioaccumulation studies, and emerging persistent organic pollutants. Cloud integration and standardized eWorkflows may facilitate harmonized global regulatory compliance.

Conclusion

The Thermo Scientific TSQ 9000 GC-MS/MS system with AEI source and Chromeleon CDS delivers reliable, sensitive, and accurate quantitation of dioxins and PCBs in food and feed, fully compliant with EU regulatory standards. Its robustness and integrated software capabilities enable efficient routine analysis, supporting food safety and public health initiatives.

References

Analysis followed EU Regulation (EU) No 252/2014, EN 1948, and EURL guidance for halogenated POPs.