Validation of a pressurized solvent extraction and GC–NCI–MS method for the low level determination of 40 polybrominated diphenyl ethers in mothers’ milk
| Autor: | Silvia Lacorte, Miriam Guillamón |
|---|---|
| Rok vydání: | 2008 |
| Předmět: |
Spectrometry
Mass Electrospray Ionization Environmental Engineering Health Toxicology and Mutagenesis Coefficient of variation Breast milk Standard solution Gas Chromatography-Mass Spectrometry Polybrominated diphenyl ethers Aluminum Oxide Halogenated Diphenyl Ethers Humans Environmental Chemistry Solid Phase Microextraction Flame Retardants Detection limit Chemical ionization Chromatography Milk Human Chemistry Extraction (chemistry) Public Health Environmental and Occupational Health Reproducibility of Results General Medicine General Chemistry Pollution Female Gas chromatography |
| Zdroj: | Chemosphere. 73:70-75 |
| ISSN: | 0045-6535 |
| DOI: | 10.1016/j.chemosphere.2008.05.021 |
| Popis: | This study reports an efficient method for the determination of 40 PBDEs from mono- to hepta-brominated in human milk. Pressurized liquid extraction (PLE) was optimized to recover PBDEs in a quantitative way using 1g of freeze dried milk. Due to the great amount of coextracted compounds, the clean-up step was optimized using alumina SPE disposable cartridges of 2 and 5 g. Whereas 2g alumina SPE failed in providing good extraction yields, all PBDEs were satisfactorily recovered using 5 g alumina SPE cartridges. Detection was performed with gas chromatography coupled to mass spectrometry with negative chemical ionization and method detection limits ranged from 0.01 to 0.05 microg kg(-1) wet weight (ww) with a good intra and inter-day variation (coefficient of variation lower than 13.4%). This method was validated by participating in an interlaboratory exercise from Quasimeme (United Kingdom), where a standard solution containing seven congeners and a certified unspiked mothers' milk were analyzed. In the standard mixture, levels between 96.915 and 570.172 microg l(-1) were quantified, whereas in certified mothers' milk, BDEs 47, 99, 100 and 154 were detected at levels from 0.010 and 0.061 microg kg(-1) ww, with an error30%. The applicability of the method was tested experimentally in five mothers' milk samples, where only BDE 47 was detected at a maximum concentration of 10.45 microg kg(-1) lipid weight (lw). PLE succeeded in extracting all PBDEs from the sample with good reproducibility although the clean-up step had to be severely performed to eliminate sample interferences such as milk lipids and proteins. |
| Databáze: | OpenAIRE |
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