Routine and robust quantification of PBDEs in food by GC-MS/MS

Significance of the Topic

The routine and robust quantification of polybrominated diphenyl ethers (PBDEs) in food is critical due to their persistence, bioaccumulation and links to adverse health effects, including carcinogenicity. As PBDEs have been widely used as flame retardants and later banned under international conventions, sensitive and reliable analytical methods are essential for food safety monitoring and regulatory compliance.

Objectives and Study Overview

This study aimed to evaluate the performance of a Thermo Scientific TSQ 9000 triple quadrupole GC-MS/MS system equipped with an advanced electron ionization (AEI) source for routine determination of 27 PBDE congeners in complex food matrices. Robustness was assessed through extended sequences of injections, tracking peak area repeatability and relative response factor (RRF) stability over hundreds of injections without maintenance.

Applied Methodology and Instrumentation

Sample extracts were injected (2 µL) via a TriPlus RSH autosampler into a TRACE 1310 GC fitted with an Instant-Connect PTV injector and an ultra-inert LinerGOLD 6 baffle liner. Chromatographic separation used a TraceGOLD TG-PBDE capillary column (15 m × 0.25 mm × 0.10 µm). Quantification employed timed-SRM transitions on the TSQ 9000 with AEI source, controlled by Chromeleon CDS 7.2 software.

Used Instrumentation:

• Thermo Scientific TSQ 9000 triple quadrupole GC-MS/MS with AEI source
• Thermo Scientific TRACE 1310 GC with Instant-Connect PTV injector
• Thermo Scientific TriPlus RSH autosampler
• TraceGOLD TG-PBDE 15 m × 0.25 mm × 0.10 µm column
• Ultra-inert LinerGOLD 6 baffle PTV liner
• Chromeleon CDS v7.2

Main Results and Discussion

Peak area repeatability for PBDEs in a fish extract (n=105 injections) showed %RSDs below 10%, with ion ratios maintained within ±30% of calibration values. Over a 320-injection sequence including 18 mid-calibration QC standards, all RRFs for 27 PBDE congeners remained within ±15% of their calibration means, with %RSDs under 10%. An example for BDE-209 yielded a mean RRF of 0.93 and %RSD of 3% over 18 QC injections. No injector liners or columns were changed, nor was any mass spectrometer maintenance or tuning required during the sequence.

Benefits and Practical Applications

The demonstrated stability and sensitivity of the TSQ 9000 AEI system enable high-throughput, accurate quantification of trace PBDEs in food samples with minimal downtime. This supports regulatory compliance, food safety laboratories and quality control units in industry and research settings.

Future Trends and Possibilities for Use

Advances may include extending this approach to other persistent organic pollutants, integrating automated sample preparation, coupling with high-resolution mass spectrometry for non-target screening, and adopting greener solvents and miniaturized injection techniques to further enhance throughput and sustainability.

Conclusion

The TSQ 9000 GC-MS/MS with AEI source and optimized GC configuration provides a robust, precise and maintenance-free platform for routine quantification of PBDEs in complex food matrices, making it well suited for long-term laboratory operations.

References

1. Hites, R. A. Polybrominated Diphenyl Ethers in the Environment and in People: A Meta-Analysis of Concentrations. Environmental Science & Technology 2004, 38, 945–956.
2. Guidance for the inventory of polybrominated diphenyl ethers (PBDEs) listed under the Stockholm Convention on POPs. United Nations Environment Programme, 2018.
3. Lamb, A.; Cojocariu, C.; Panton, S. Fast, Ultra-Sensitive Analysis of PBDEs in Food Using Advanced GC-MS/MS Technology. Thermo Scientific Application Note 10674, October 2018.
4. Fernandes, A.; White, S.; D’Silva, K.; Rose, M. Simultaneous Determination of PCDDs, PCDFs, PCBs and PBDEs in Food. Talanta 2004, 63, 1147–1155.
5. Thermo Fisher Scientific. Timed SRM Technical Note: Multitarget Compound Analysis. 2009.