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

FONTANA, ARIEL; WUILLOUD, RODOLFO G.; MARTINEZ, LUIS D.; ALTAMIRANO, JORGELINA C.

JOURNAL OF CHROMATOGRAPHY - A

Elsevier

Año: 2009 vol. 1216 p. 147 - 153

0021-9673

A simple, efficient, innovative and environmentally friendly analytical techniquewas successfully applied for 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 literature in 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 by gas chromatography-mass spectrometry (GC-MS). The extraction/preconcentration technique is based on ultrasound-assisted emulsification-microextraction (USAEME) of a water-immiscible solvent in an aqueousmedium. Several variables including, solvent type, extraction time, extraction temperature and matrix modifierswere studied and optimized over the relative response the target analytes. Chloroformwas used as extraction solvent in the USAEME technique.Under optimum conditions, the target analyteswere quantitatively extracted achieving enrichment factors (EF) higher than 319. The detection limits (LODs) of the analytes for the preconcentration of 10 mLsample volume were within the range 1¨C2 pg mL−1. The relative standard deviations (RSD) for five replicates at 10 pg mL−1 concentration level were <10.3%. The calibration graphs were linear within the concentration range of 5-5000 pg mL−1 for BDE-47 and BDE-100; and 5-10,000 pg mL−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 pg mL−1). Recovery values were 96%, which showed a successful robustness of the analytical methodology for determination of pictogram per milliliter of PBDEs in water samples. Significant quantities of PBDEs were not found in the analyzed samples.