Determination of Polychlorinated Dibenzo-p-dioxins and Dibenzofurans (PCDD/Fs) in Foodstuffs and Animal Feed Using a Triple Quadrupole GCMS-TQ8040 System with Smart MRM Transforms Laboratory Analysis

Importance of the Topic

Polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) are persistent organic pollutants with high toxicity and the capacity to bioaccumulate in food chains. Regulatory agencies such as the European Union have established strict maximum levels for PCDD/Fs in foodstuffs and animal feed, making reliable monitoring methods essential for food safety and public health.

Study Objectives and Overview

This report describes the development and validation of a sensitive, selective, and reproducible method for quantifying 17 2,3,7,8-substituted PCDD/F congeners in food and feed. A Shimadzu GCMS-TQ8040 triple quadrupole system coupled with Smart MRM technology was employed to meet performance requirements comparable to high-resolution GC/HRMS methods mandated by EU regulations.

Methodology and Instrumentation

The analytical procedure combines modified US EPA Method 1613B sample preparation with Smart MRM-enhanced GC–MS/MS analysis:

• Accelerated solvent extraction of homogenized samples spiked with 13C-labeled surrogates.
• Multi-stage cleanup using acidic/basic silica, alumina, and carbon chromatography.
• Addition of 13C-labeled internal standards prior to analysis.
• GC–MS/MS analysis in multiple reaction monitoring mode with automated transition and collision energy optimization.

Used Instrumentation

• Shimadzu GCMS-TQ8040 triple quadrupole mass spectrometer with OFF-AXIS ion optics.
• DB-5MS capillary column (60 m × 0.25 mm × 0.25 µm).
• Splitless injector (290 °C) and argon collision gas (150 kPa).
• Smart MRM software for retention-time synchronized MRM and optimized dwell/loop settings.

Main Results and Discussion

The method delivered:

• Full chromatographic separation of all 17 target congeners within 60 min.
• Detection limits as low as 10 fg on-column for 2,3,7,8-TCDD, with linear calibration from 0.1 to 200 ng/mL (R² > 0.999).
• Intra- and interday repeatability with RSD < 15% for low-level standards.
• Real-sample analysis of fish oil and milk yielding TEQ values (29.5 pg WHO-TEQ2005/g fat and 1.38 pg WHO-TEQ2005/g fat, respectively) consistent with HRGC/HRMS results.

Benefits and Practical Applications

This triple quadrupole GC–MS/MS approach offers a rapid, cost-effective alternative to high-resolution mass spectrometry for routine PCDD/F screening and quantitation, fully compliant with EU legislation. Smart MRM significantly reduces method development time and enhances laboratory throughput.

Future Trends and Potential Applications

Emerging developments may include:

• Expansion of Smart MRM databases to cover additional environmental contaminants.
• Integration of automated sample prep and data analysis workflows.
• Development of multi-class methods encompassing PCDD/Fs, dioxin-like PCBs, and other regulated pollutants.

Conclusion

The Shimadzu GCMS-TQ8040 with Smart MRM delivers the sensitivity, linearity, and precision required for robust PCDD/F analysis in food and feed. It represents a practical solution for routine regulatory monitoring in compliance with EU standards.

Reference

1. Institute of Medicine. Dioxins and dioxin-like compounds in the food supply: Strategies to decrease exposure. The National Academies Press, Washington DC, 2003.
2. Commission Regulation (EU) No. 589/2014 of 2 June 2014 laying down methods of sampling and analysis for the control of levels of dioxins, dioxin-like PCBs and non-dioxin-like PCBs in certain foodstuffs.
3. Commission Regulation (EU) No. 709/2014 of 20 June 2014 amending Regulation (EC) No. 152/2009 on determination of dioxins and PCBs.
4. US EPA Method 1613B: Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution HRGC/HRMS, 1997.
5. Wang P, Zhang Q, Wang Y et al. Evaluation of extraction techniques for PCBs and PBDEs in soil and fish. Anal. Chim. Acta. 2010;663(1):43–48.