Ultrasound-assisted leaching-dispersive solid-phase extraction followed by liquid–liquid microextraction for the determination of polybrominated diphenyl ethers in sediment samples by gas chromatography–tandem mass spectrometry

• Published in: Talanta (Oxford) 2010-06, Vol.82 (1), p.359-366
• Main Authors: Fontana, Ariel R., Lana, Nerina B., Martinez, Luis D., Altamirano, Jorgelina C.
• Format: Article
• Language: English
• Subjects: Analytical chemistry; Chemistry; Chromatographic methods and physical methods associated with chromatography; Dispersive liquid–liquid microextraction; Environmental Pollutants - analysis; Environmental Pollutants - isolation & purification; Exact sciences and technology; Gas chromatographic methods; Gas Chromatography-Mass Spectrometry - methods; Gas chromatography–mass spectrometry; Geologic Sediments - chemistry; Halogenated Diphenyl Ethers - analysis; Halogenated Diphenyl Ethers - isolation & purification; Linear Models; Polybrominated diphenyl ethers; Reproducibility of Results; Sediment analysis; Solid Phase Extraction - methods; Solvents - chemistry; Spectrometric and optical methods; Temperature; Time Factors; Ultrasonics; Ultrasound-assisted leaching-dispersive solid-phase extraction
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2010.04.050

Ultrasound-assisted leaching-dispersive solid-phase extraction followed by dispersive liquid–liquid microextraction (USAL-DSPE-DLLME) technique has been developed as a new analytical approach for extracting, cleaning up and preconcentrating polybrominated diphenyl ethers (PBDEs) from sediment samples prior gas chromatography–tandem mass spectrometry (GC–MS/MS) analysis. In the first place, PBDEs were leached from sediment samples by using acetone. This extract was cleaned-up by DSPE using activated silica gel as sorbent material. After clean-up, PBDEs were preconcentrated by using DLLME technique. Thus, 1 mL acetone extract (disperser solvent) and 60 μL carbon tetrachloride (extraction solvent) were added to 5 mL ultrapure water and a DLLME technique was applied. Several variables that govern the proposed technique were studied and optimized. Under optimum conditions, the method detection limits (MDLs) of PBDEs calculated as three times the signal-to-noise ratio (S/N) were within the range 0.02–0.06 ng g −1. The relative standard deviations (RSDs) for five replicates were