Method development and validation for the determination of polybrominated diphenyl ether congeners in Brazilian aquatic sediments

An analytical method was developed and validated for the determination of nine PBDE congeners (BDE 28, 47, 66, 85, 99, 100, 138, 153 and 154) in aquatic sediment samples using ultrasonic solid-liquid extraction (acetone:n-pentane 1:1v/v) followed by gas chromatography coupled with electron capture d...

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Bibliographic Details
Published in:Microchemical journal 2017-07, Vol.133, p.43-48
Main Authors: Annunciação, Daniel Luiz Rodrigues, Almeida, Fernanda Vasconcelos, Sodré, Fernando Fabriz
Format: Article
Language:English
Subjects:
Brazilian waters
Brominated flame retardants
Emerging contaminants
Polybrominated diphenyl ethers
Sediment
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Summary:An analytical method was developed and validated for the determination of nine PBDE congeners (BDE 28, 47, 66, 85, 99, 100, 138, 153 and 154) in aquatic sediment samples using ultrasonic solid-liquid extraction (acetone:n-pentane 1:1v/v) followed by gas chromatography coupled with electron capture detection. Values for LOD varied between 0.58 and 0.96ngg−1 while LOQ ranged from 1.92 to 3.21ngg−1. Fortified and certified reference sediments were investigated for method accuracy and precision. Recovery, varying from 87.7±6.6% (BDE-138) to 98.7±1.4% (BDE-28), was influenced by strong hydrophobic interactions between analytes and the sediment matrix. The validated method was successfully used to assess PBDE levels in a Brazilian sediment sample collected at the Paranoá Lake, in Brasília (Brazil). Results revealed environmental concentrations above the reported LOQ for two of the nine PBDE congeners being the BDE-66 the most prevalent (8.1±0.4ngg−1) followed by BDE-47 (2.51±0.02ngg−1). Further investigations are still needed to evaluate the contamination pattern of PBDE in Brazilian sediments, notably in urbanized regions. •An ultrasonic solid-liquid extraction method was developed for determination of PBDE in aquatic sediments.•Method accuracy and precision were investigated using fortified and certified reference sediments.•BDE-66 and BDE-47 were found in sediment from Lake Paranoá, an artificial lake located in the capital of Brazil.•This work is the first investigation of PBDEs in Brazilian sediments.
ISSN:0026-265X
1095-9149
DOI:10.1016/j.microc.2017.03.009