Solid-phase extraction combined with dispersive liquid–liquid microextraction for the determination for polybrominated diphenyl ethers in different environmental matrices

• Published in: Journal of Chromatography A 2009-03, Vol.1216 (12), p.2220-2226
• Main Authors: Liu, Xiujuan, Li, Jianwang, Zhao, Zhixu, Zhang, Wei, Lin, Kuangfei, Huang, Changjiang, Wang, Xuedong
• Format: Article
• Language: English
• Subjects: Analysis methods; Analytical chemistry; Animal, plant and microbial ecology; Applied ecology; Applied sciences; Biological and medical sciences; Chemistry; Chromatographic methods and physical methods associated with chromatography; Ecotoxicology, biological effects of pollution; Effects of pollution and side effects of pesticides on plants and fungi; Exact sciences and technology; Fundamental and applied biological sciences. Psychology; Gas chromatographic methods; Gas chromatography–electron capture detection (GC–ECD); Natural water pollution; Plant sample; Pollution; Polybrominated diphenyl ethers (PBDEs); Solid-phase extraction combined with dispersive liquid–liquid microextration (SPE–DLLME); Water sample; Water treatment and pollution
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2008.12.092

An analytical method, solid-phase extraction combined with dispersive liquid–liquid microextration (SPE–DLLME), was established to determine polybrominated diphenyl ethers (PBDEs) in water and plant samples. After concentration and purification of the samples in LC-C18 column, 1.0-mL elution sample containing 22.0 μL 1,1,2,2-tetrachloroethane was injected rapidly into the 5.0-mL pure water. After extraction and centrifuging, the sedimented phase was injected rapidly into gas chromatography with electron-capture detection (GC–ECD). For water samples, enrichment factors (EFs) are in the range of 6838–9405 under the optimum conditions. The calibration curves are linear in the range of 0.1–100 ng L −1 (BDEs 28, 47) and 0.5–500 ng L −1 (BDEs 100, 99, 85, 154, 153). The relative standard deviations (RSDs) and the limits of detection (LODs) are in the range of 4.2–7.9% ( n = 5) and 0.03–0.15 ng L −1, respectively. For plant samples, RSDs and LODs are in the range of 5.9–11.3% and 0.04–0.16 μg kg −1, respectively. The relative recoveries of well, river, sea, leachate, and clover samples, spiked with different levels of PBDEs, are 66.8–94.1%, 72.2–100.5%, 74.5–110.4%, 62.1–105.1%, 66.1–91.7%, 62.4–88.9%, and 64.5–83.2%, respectively. The results show that SPE–DLLME is a suitable method for the determination of PBDEs in water and plant samples.