Highly sensitive determination of polybrominated diphenyl ethers in surface water by GC coupled to high‐resolution MS according to the EU Water Directive 2008/105/EC

• Published in: Journal of separation science Vol. 37; no. 1-2; pp. 69 - 76
• Main Authors: Barco‐Bonilla, Nieves, Plaza‐Bolaños, Patricia, Tarifa, Noelia Ma Valera, Romero‐González, Roberto, Martínez Vidal, José Luis, Frenich, Antonia Garrido
• Format: Journal Article
• Language: English
• Published: Weinheim Blackwell Publishing Ltd 2014; Wiley; Wiley Subscription Services, Inc
• Subjects: Analysis methods; Analytical chemistry; Applied sciences; Bromination; Chemical contaminants; Chemistry; Chromatographic methods and physical methods associated with chromatography; Environmental Monitoring - legislation & jurisprudence; Environmental Monitoring - methods; environmental quality; Environmental quality standards; European Union; Exact sciences and technology; Fire resistant materials; flame retardants; Flame Retardants - analysis; Fresh Water - chemistry; Gas chromatographic methods; Gas Chromatography-Mass Spectrometry - methods; GC coupled to high-resolution MS; Halogenated Diphenyl Ethers - analysis; laws and regulations; Magnetic sector; Mass spectrometry; Natural water pollution; Pollution; Polybrominated diphenyl ethers; Sensitivity and Specificity; Surface water; toxicity; Water Pollutants, Chemical - analysis; Water Pollution, Chemical - analysis; Water Pollution, Chemical - legislation & jurisprudence; Water treatment and pollution; Validation; Solid phase extraction; Coupled method; Flame retardant; Chemical enrichment; Persistent organic pollutant; Gas chromatography; Polybrominated diphenyl ethers; Sample preparation; European directive; Polybromo diphenyl ether; GC coupled to high-resolution MS; Surface water; Bromine Organic compounds; Water pollution; Environmental quality standards; Magnetic sector; Mass spectrometry; Quantitative analysis
• ISSN: 1615-9306; 1615-9314
• DOI: 10.1002/jssc.201300757

The analysis of brominated flame retardants, such as polybrominated diphenyl ethers (PBDEs), has received increased interest because of their toxicity and ubiquity. According to European Union Directive 2008/105/EC, the development of highly sensitive and selective methods capable of determining PBDEs at low concentration levels (<0.5 ng/L) is necessary. In this work, an SPE method was developed for the analysis of the six PBDEs (BDE‐28, BDE‐47, BDE‐99, BDE‐100, BDE‐153, BDE‐154) specified by the aforementioned directive in surface waters. The analyses were performed by GC coupled to magnetic sector high‐resolution MS. The conditions were also optimized to detect the target compounds in water samples at concentrations below the environmental quality standards established by European legislation. The validated method provided adequate linearity (determination coefficient, R² ≥ 0.9960), recovery (101–120%, except for BDE‐47 at 5 ng/L, 127%), and precision values (RSD < 20%) at two fortification levels (0.2 and 5 ng/L). The method showed LODs and LOQs ranging from 0.02 to 0.05 and from 0.05 to 0.1 ng/L, respectively. The method was applied in surface water samples, allowing the determination of these compounds at the limits established by current legislation.