Simple approach based on ultrasound-assisted emulsification-microextraction for determination of polibrominated flame retardants in water samples by gas chromatography-mass spectrometry

FONTANA, A.R.,; WILLOUD, R.G; MARTINEZ, L. D; ALTAMIRANO, J.C.

JOURNAL OF CHROMATOGRAPHY - A

Elsevier

Año: 2009 p. 147 - 153

0021-9673

A simple, efficient, innovative and environmentally friendly analytical techniquewas successfully appliedfor the first time for the extraction and preconcentration of polybrominated diphenyl ethers (PBDEs)from water samples. The PBDEs selected for this work were those most commonly found in the literaturein natural water samples: 2,2,4,4-tetraBDE (BDE-47), 2,2,4,4,5-pentaBDE (BDE-99), 2,2,4,4,6-pentaBDE(BDE-100) and 2,2,4,4,5,5-hexaBDE (BDE-153). The extracted PBDEs were separated and determined bygas chromatography–mass spectrometry (GC–MS). The extraction/preconcentration technique is based onultrasound-assisted emulsification-microextraction (USAEME) of a water-immiscible solvent in an aqueousmedium.Several variables including, solvent type, extraction time, extraction temperature and matrixmodifierswere studied and optimized over the relative response the target analytes. Chloroformwas usedas extraction solvent in the USAEMEtechnique.Under optimum conditions, the target analyteswere quantitativelyextracted achieving enrichment factors (EF) higher than 319. The detection limits (LODs) of theanalytes for the preconcentration of 10mLsample volumewere within the range 1–2 pgmL−1. The relativestandard deviations (RSD) for five replicates at 10 pgmL−1 concentration level were <10.3%. The calibrationgraphs were linear within the concentration range of 5–5000 pgmL−1 for BDE-47 and BDE-100; and5–10,000 pgmL−1 for BDE-99 and BDE-153, respectively. The coefficients of estimation were ≥0.9985.Validation of the methodology was performed by standard addition method at two concentration levels(10 and 50 pgmL−1). Recovery values were ≥96%, which showed a successful robustness of the analyticalmethodology for determination of picogramper milliliter of PBDEs inwater samples. Significant quantitiesof PBDEs were not found in the analyzed samples.© 2008 Elsevier B.V. All rights reserved.