Polybrominated Diphenyl Ethers, more commonly referred to by the acronym PBDEs, are widely used fire retardants in many consumer items, including: polyurethane foam found in furniture and carpeting, home electronics and other textiles. In 2004, use of Penta-BDEs and Octa-BDEs were banned and production was phased out at this time. However, items containing these chemicals still exist.

Now, PBDEs are under investigation in animal models as agents interfering with immunological, embryonic development and endocrine functions.

Low population background levels have favored analysis by high resolution mass spectrometry (HRMS), limiting this analysis to highly specialized laboratories. This presentation describes a rapid solvent free extraction of PBDEs from a small serum sample (0.25 ml), with processing time of 2-3 hours using solid phase extraction of analytes from matrix (GERSTEL Twister® stir bar sorptive extraction).  Gas chromatographic separation with electron capture negative ion mass selective detection (GC/ MSD-ECNI-SIM) produces quantitative results with detection limits fit for purpose using instrumentation readily available in most analytical laboratories.

Results of Experiment – PBDE Analysis in Human Blood Serum by GERSTELTwister© Stir-bar Sorptive Extraction Technique and GC/MS-ECNI-SIM – Conducted by Colin Johnson, Paul R. Loconto, Michael O’Keefe, Bonita Taffe:

-Good separation of congeners was achieved with this method and background levels were acceptable.

-This method uses a 6 point calibration curve in serum for analysis of BDE congeners, R2 ≥0.99.

-Quality control limits using NIST SRM 1958 for QH.

-The LOD for each congener measured is less than 0.2 ppb

-No interference with extraction of BDEs by the SBSE was detected from other analytes in the NIST SRM 1958 (which contains PCBs, pesticides and other organochlorine metabolites).

-Measured analytes were averaged and compared with NIST reported levels. All BDEs except BDE 85 were within 2SD of reported values; BDE 85 was within 3SD. Measured values for PBB 153 were lower than NIST reported values.

-Accuracy and Precision were measured using replicates of the Arctic Monitoring and Proficiency Program (AMAP) samples as well as the NIST SRM and compared to proficiency program participant results.

Conclusion

-A rapid analytical method which uses 0.25 ml of human serum has been validated for PBDEs

-This method uses GERSTEL Twister SBSE extraction. A procedure for enhanced BDE background elimination and cleanup for Stir-bar re-use has been developed.

-The method has been demonstrated to be both accurate and precise at concentration levels found in human subpopulations

-PBDE-47 and 99 are generally demonstrated in analysis. This study demonstrates ways to reduce high environmental background levels without extreme measures (clean room preparation).

-The limit of detection for this method for each congener is less than 0.2 ppb. This method could be used for population screening to identifying more highly exposed subpopulations.

If you have any questions about the GERSTEL products and methods described in this post, GERSTEL, or any other GERSTEL products, technologies or techniques, please contact GERSTEL USA by calling 1-800-413-8160 or click here today!

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Sources:

PBDE Analysis in Human Blood Serum by GERSTEL Twister© Stir-bar Sorptive Extraction Technique and GC/MS-ECNI-SIM by Colin Johnson, Paul R. Loconto, Michael O’Keefe, Bonita Taffe