This method is for the determination of polybrominated diphenyl ethers (PBDEs) from aqueous, solid, tissue, and multi-phase matrices by high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS).
Aqueous samples are extracted using solid-phase extraction (SPE), separatory funnel extraction (SFE), or continuous
liquid/liquid extraction (CLLE). Solid, semi-solid, and multi-phase samples (excluding tissue) are extracted using a Soxhlet/Dean-Stark extractor. Fish and other tissue is dried with anhydrous sodium sulfate and extracted for 18-24 hours using methylene chloride in a Soxhlet extractor. Lipid content should also be determined for tissue samples. Tissue sample extracts are cleaned up using an anthroopogenic isolation column. All sample extracts are cleaned up using and acid/base column and gel permeation, silica gel, and/or Florisil or alumina chromatography, as required.
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Hold Times, Preservatives, Preps, Collection, Analytical & Documentation | |
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Holding Time: | Aqueous samples are good for up to one year if properly preserved and stored in the dark at <6°C. Solid, semi-solid, tissue and other matrices may be stored for up to one year if stored in the dark at <-10°C. |
Preservatives: | If residual chlorine is present, add 80mg of sodium thiosulfate per L of aqeuous sample. Ship all samples at <6°C. Store aqueous samples at <6°C and solid, semi-solid, tissue and other matrices at <-10°C. |
Required Preps: | 1L Amber glass bottle with Teflon-lined lid |
Collection Method: | Grab sampling |
Analytical Methodology: | HRGC/HRMS |
Documentation: | 1614 |
* The analytes and detection limits listed for each method represent the typical detection limits and analytes reported for that particular method. Keep in mind that analyte lists may vary from laboratory to laboratory. Detection limits may also vary from lab to lab and are dependent upon the sample size, matrix, and any interferences that may be present in the sample.