Instrument Performance Standards: A new Concept for fast Routine Performance Checks and Method Development in GC/MS Analysis of Dioxins and Furans

Significance of the Topic

The routine monitoring of dioxins and furans at femtogram levels is critical due to their high toxicity, persistence and bioaccumulative nature. Regulatory limits in food and feed require analytical methods with high sensitivity and reproducibility. Fast and reliable instrument performance checks support compliance with EU screening (RSD <30%) and confirmation (RSD <15%) criteria and help prevent public health incidents and economic losses.

Objectives and Study Overview

This study presents a concept and practical tool for rapid evaluation of GC/HRMS performance in dioxin and furan analysis. Two dedicated performance standards are introduced: one for sensitivity and linearity across six concentration levels (2–100 fg/µL) and another for reproducibility at a fixed concentration (5 pg/µL). The approach enables assessment of detection limits, isotope ratio accuracy, signal-to-noise and calibration in a single injection per standard.

Methodology and Used Instrumentation

All measurements were carried out on a Thermo Scientific DFS high-resolution magnetic sector mass spectrometer coupled to a Trace GC Ultra with a TriPlus autosampler. Two TR-Dioxin 5ms columns (30 m × 0.25 mm × 0.1 µm and 60 m × 0.25 mm × 0.25 µm) with SSL injector were used. Sensitivity and reproducibility standards were developed at Thermo Fisher Scientific POPs Application Lab (Bremen) and produced by Wellington Laboratories (Canada), now commercialized by Campro Scientific (Germany).

Main Results and Discussion

Using the sensitivity standard, linear calibration curves with R² ≥ 0.9991 were obtained from 2 to 100 fg/µL. Signal-to-noise ratios exceeded 200:1 at 20 fg and 50:1 at 10 fg. The reproducibility standard yielded RSDs of 3–5% at 100 fg, 4–7% at 20 fg and 7–10% at 10 fg for individual congeners. Single-injection isotope ratios and relative peak areas matched expected values. These data confirm that single-injection performance standards efficiently characterize instrument sensitivity and reproducibility without multiple dilutions.

Benefits and Practical Applications

• Rapid instrument qualification prior to sample analysis
• Informed decisions on method optimization (injection volume, sampling points, dwell times)
• Determination of sample processing requirements to meet EU limits
• Efficient maintenance scheduling to restore performance

Future Trends and Applications

Integrating automated performance checks into laboratory information systems could further accelerate quality control. Expanding standards to cover additional congeners or matrices will increase method robustness. Emerging HRMS technologies may allow multiplexed evaluation of broader compound classes in a single run.

Conclusion

The dual performance standard concept provides a fast, reliable and reproducible approach to assess GC/HRMS performance for dioxin and furan analysis. By consolidating sensitivity and reproducibility checks into single injections, laboratories can ensure compliance with stringent regulatory criteria and optimize analytical workflows.

References

1. Commission Regulation (EC) No. 1883/2006
2. Commission Regulation (EC) No. 199/2006, amending Regulation (EC) No. 466/2001
3. Campro Scientific product information (www.campro.eu)