PBDE analysis

Polybrominated Diphenyl Ethers. Information on the relative importance of different routes of exposure to PBDEs is limited. Data on the concentrations of PBDEs in foods, collected using a market-basket approach, are needed to determine concentrations of PBDEs in foods consumed by the general population. Data on the PBDE concentrations in foods grown in contaminated areas, particularly in the vicinity of hazardous waste sites, are also needed. Data on congener-specific PBDE analysis of food, especially plant products, would be useful. More monitoring data on the concentrations of total PBDEs as well as conquers in air in remote, rural, urban, and areas near hazardous waste sites and incinerators are needed. Data on PBDE concentrations in finished drinking water nationwide would be helpful. 

In El-MS, the major ions formed from PBDEs are the and the [M — 2Br], which can be used for its identification and quantitation. This ionization technique facilitates the analysis of BDE congeners in the presence of possible coeluted compounds (such as PCBs). EI-LRMS is not routinely used for the PBDE analysis, because of its relatively low sensitivity, especially for the analysis of higher brominated BDE congeners (hepta- to deca-DBE). However, this ionization mode allows the acquisition of full scan spectra, thus offering a multiple choice in ion selection than ECNI mode. Yet, ECNI is more selective towards aromatic brominated compounds. 

For PBDE analyses, the complexity of sludge matrix implies the use of multi-step purification methods. Sludge extracts contain relatively large amounts of elemental sulfur, which would disturb the GC analysis, and must be removed. 

In the case of deca-BDE mixture, the formation of less brominated compounds was not detected for any of the samples (time of degradation corresponding to 24, 36, 60, 84 and 182 h). Regarding octa-BDE and penta-BDE mixtures, the analysis of samples at time 168 h did not detect an increase in concentration for any of the components present in each of the mixtures or the formation of any PBDE not present in the original composition of both mixtures. Therefore, the results obtained for the three mixtures demonstrated that the PBDEs degradation by the fungus does not follow the reductive debromination pathway, which is logical because this... 

A rapid and simple method for PBDE and HBCD determinations in sediment and fish samples was used. The analytical method was based in selective pressurized liquid extraction (SPLE) [21] without further cleanup step and analysis by gas chromatography coupled to mass spectrometry (GC-MS), working with negative ion chemical ionization (NCI) [22, 23],... 

Xu T, Cho IK, Wang D, Rubio FM, Shelver WL, Gasc AME, Li J, Li QX (2009) Suitability of magnetic particle immunoassay for the analysis of PBDEs in Hawaiian euryhaline fish and crabs in comparison with gas chromatography/electron capture detection-ion trap mass spectrometry. Environmental Pollution 157 417 22... 

To be added in cases of indications for relevance and bioavailability In vivo bioassays with relevant exposure conditions, routes and endpoints Prolonged ELS and metamorphosis In vivo bioassays with sediment extracts In vitro bioassays specific mechanisms Internal effect levels Specific chemicals (e.g. PFACs, HBCDs, PBDEs) ELS not longer than free feeding Chemicals that only are toxic in high concentration (narcotics, nanoparticles) Chemical analysis of lipophillic POPs in water... 

Methods for the detemination of organobromine compounds such as PBBs and PBDEs generally consist of the following steps extraction of the analyte from the sample matrix clean-up to remove interfering compounds and analysis (separation and quantitation). The primary method of analysis is GC coupled with ECD or MS. Analytical methods have been developed for the determination of PBBs and PBDEs in blood or serum, urine, feces, adipose tissue, liver, and breast milk. The methods for determining PBB and PBDE residues in biological samples are given in Tables 7-1 and 7-2, respectively. 

ECD = electron capture detection GC = gas chromatography GPC = gel permeation chromatography HRMS = high resolution mass spectrometry LC = liquid chromatography MS = mass spectrometry NAA = neutron activation analysis NCI = negative chemical ionization PBDEs = polybrominated diphenyl ethers... 

It would be helpful to develop data determining the accuracy of PBDE determinations (e.g., percent recovery) in environmental samples. Methods for determining degradation products and metabolites of PBDE are needed. There is no information in the literature of detectable biodegradation of PBDEs in the environment under aerobic or anaerobic conditions. The analysis of PBDE pyrolysis degradation products, such as polybrominated dibenzo-p-dioxins and dibenzofurans (PBDD/Fs), is often disturbed by the presence of PBDEs. Ebert et al. (1999) demonstrated that by using a Florisil column ina sample clean-up process, almost complete separation of PBDEs and PBDD/Fs is achieved before analysis by GC-MS. 

She J, Wrinkler J, Visita P, et al. 2000. Analysis of PBDEs in seal blubber and human breast adipose tissue samples. Organohalogen Compoimds 47 53-56. 

During the analysis of PBDE in the particle phase of atmosphere samples from various sites in the United States, Hoh et al. [60] noticed a significant, unknown, bromine-containing gas chromatographic (GC) peak in some samples. To identify this unknown substance, full-scan mass spectra were obtained in both electron-impact and electron-capture negative ionization modes. Based on this analysis, it was suspected that this GC peak might be... 

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