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

FONTANA, A.; LANA, N. B.; MARTINEZ, L.; ALTAMIRANO, J.

TALANTA

ELSEVIER SCIENCE BV

Lugar: Amsterdam; Año: 2010 vol. 82 p. 359 - 366

0039-9140

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, 1mL acetone extract (disperser solvent) and 60 L carbon tetrachloride (extraction solvent) were added to 5mL 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