INVESTIGADORES
ALTAMIRANO Jorgelina Cecilia
artículos
Título:
Simple approach based on ultrasound-assisted emulsification-microextraction for determination of polibrominated flame retardants in water samples by gas chromatography-mass spectrometry
Autor/es:
FONTANA, ARIEL R.; WUILLOUD, RODOLFO G.; MARTINEZ, LUIS D.; ALTAMIRANO, JORGELINA C.
Revista:
JOURNAL OF CHROMATOGRAPHY - A
Editorial:
Elsevier
Referencias:
Lugar: Amsterdam; Año: 2009 vol. 1216 p. 147 - 153
ISSN:
0021-9673
Resumen:
A simple, efficient, innovative and environmentally friendly analytical
technique was 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 aqueous medium. Several variables including, solvent type,
extraction time, extraction temperature and matrix modifiers were
studied and optimized over the relative response the target analytes. Chloroform
was used as extraction solvent in the USAEME technique. Under optimum
conditions, the target analytes were quantitatively extracted achieving
enrichment factors (EF) higher than 319. The detection limits (LODs)
of the analytes for the preconcentration of 10 mL sample volume were
within the range 1 2 pg mL-1. The relative standard deviations (RSD) for 5 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 5-10000 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 picogram per milliliter of PBDEs in water samples. Significant quantities of PBDEs were not found in the analyzed samples.