High Efficiency, Quantitative Dioxins Screening at the Level of Interest in Feed and Food using Advanced GC-MS/MS

Význam tématu

Dioxins and dioxin-like compounds pose significant health risks through bioaccumulation in the food chain, chiefly from animal-derived products.
Regulatory authorities enforce strict maximum levels and extensive monitoring to protect consumers and avoid economic and political fallout.

Cíle a přehled studie / článku

This study evaluates the performance of the Thermo Scientific TSQ Quantum XLS Ultra GC-MS/MS platform for high-efficiency screening of PCDD/Fs in feed and food.
It benchmarks screening results against the gold standard GC-HRMS (Thermo Scientific DFS) under EU regulation thresholds.

Použitá metodika a instrumentace

Extraction and Clean-up:

• Sample extraction and multi-step clean-up following validated protocols, targeting a maximum of 3 g fat for low LOQ.

Instrumentation and Conditions:

• GC-MS/MS system: TSQ Quantum XLS Ultra with EI source (40 eV, 250 °C, 50 µA).
• MS/MS parameters: Q2 argon collision (1.5 mTorr, 22 V), Q1/Q3 resolution at 0.7 amu.
• PTV injection: 5 µL toluene, 100 °C ramped to 340 °C.
• GC column: DB-5MS (60 m × 0.25 mm, 0.25 µm) with temperature program from 120 °C to 285 °C.
• Confirmatory analysis: Thermo Scientific DFS high resolution MS.

Hlavní výsledky a diskuse

Sensitivity and Selectivity:

• Achieved detection at 0.13 pg/g fat for 2,3,7,8-TCDD with 12% CV across five injections.
• Consistent SRM chromatograms at lowest calibration levels, enabling precise quantification.

Ion Ratio Confirmation:

• Measured ion ratios matched theoretical values within ±15% tolerance, ensuring reliable identity confirmation.

Quantitative Performance:

• Isotope dilution quantification provided real TEQ values and recoveries of 83–110% with RSDs mostly below 20% for 42 food samples.

Screening Efficiency:

• WHO-PCDD/F-TEQ results correlated strongly with HRMS data down to ~0.5 pg/g level, indicating low false negatives and high selectivity.

Přínosy a praktické využití metody

• High-throughput screening reduces reliance on time-intensive HRMS confirmatory analyses.
• Retention of isotope dilution and congener profiling supports accurate TEQ calculation and monitoring trends.
• Compliance with EU regulations for screening minimizes non-compliant sample releases.

Budoucí trendy a možnosti využití

• Expansion to other persistent organic pollutants and further multi-residue applications.
• Integration with automated sample preparation and miniaturized platforms to increase throughput.
• Potential coupling with rapid bioassays for tiered screening strategies.

Závěr

The TSQ Quantum XLS Ultra GC-MS/MS demonstrates robust sensitivity, selectivity, and quantitative accuracy for dioxin screening in compliance with EU regulations.
Its strong agreement with GC-HRMS confirmatory data and predictable ion ratios establish it as a reliable, efficient tool for routine feed and food safety testing.

Reference

1. European Food Safety Authority; Results of the monitoring of dioxin levels in food and feed. EFSA Journal 2010;8(3):1385.
2. Commission Regulation (EC) No 152/2009 and No 1883/2006.