Analysis of Dioxins and Furans on a Xevo G2-XS QTof with APGC Using a QuEChERS Extraction Method

Significance of the Topic

Dioxins and furans are persistent organic pollutants with serious health implications and strict regulatory controls. Rapid, cost-effective detection in environmental samples is vital for site assessment and remediation projects.

Objectives and Study Overview

This work aimed to develop a faster, more economical method for quantifying dioxins and furans in sediment, using a QuEChERS extraction approach combined with Atmospheric Pressure GC and high resolution QTof mass spectrometry. The goal was to meet or exceed EPA Method 1613 performance criteria while improving sample throughput and reducing solvent use.

Methodology and Instrumentation

The study employed a modified QuEChERS protocol: sediment samples fortified with 13C-labeled standards were extracted into acetonitrile–water, salted out, and the organic phase solvent-exchanged into hexane. Cleanup was achieved using carbon columns. Analysis used a Waters Xevo G2-XS QTof fitted with an APGC source, paired with a Restek Rtx-Dioxin2 GC column (20–40 m). MassLynx software controlled data acquisition. Instrumental parameters were optimized for high flow rates and varied column lengths to balance speed and resolution.

Main Results and Discussion

Calibration of 2,3,7,8-TCDD over 0.5–200 pg showed excellent linearity (R2 = 0.9993). Comparison with NIST 1944 reference material indicated equal or superior accuracy for critical congeners compared to a magnetic sector HRMS. Studies of flow rates (0.5–3 mL/min) and column lengths (20–40 m) demonstrated that higher flows and shorter columns significantly reduced runtime (<15 min/sample) with minimal loss in separation, even for challenging isomer pairs.

Benefits and Practical Applications

• Sample throughput increased by over 15× compared to traditional magnetic sector methods
• Reduced sample preparation time and solvent consumption
• Less demand on specialist operators while maintaining EPA Method 1613 compliance
• Flexible platform enabling both targeted and non-targeted screening of emerging contaminants

Future Trends and Possibilities

Advances may include integration of automated QuEChERS workflows, expansion to other persistent organic pollutants, and coupling APGC-QTof with supplementary ionization modes for broader non-target analysis. High throughput platforms will support large-scale monitoring and rapid decision making in environmental assessment.

Conclusion

The combined QuEChERS extraction and APGC-QTof approach provides a robust, high-throughput method for dioxin and furan analysis in sediment. It achieves regulatory performance while reducing costs and analysis time, offering a practical alternative to conventional HRMS workflows.

Reference

1. Dioxins and Furans Factsheet. EPA. 2. Stockholm Convention on Persistent Organic Pollutants. 3. Reiner EJ. Mass Spectrum Techniques. Mass Spectrom Rev. 2010;29:526–559. 4. Perelo LW. J Hazard Mater. 2010;177:81–89. 5. Anastassiades et al. QuEChERS method. J AOAC Int. 2003;86:412–431. 6. Haimovici L et al. Anal Bioanal Chem. 2016;408:4043–4054. 7. Richman L et al. J Environ Prot. 2016;7:453.