Dispersive solid-phase extraction followed by liquid-liquid microextraction for extraction and preconcentration of PBDEs from sediment samples prior gas chromatography-mass spectrometry

ALTAMIRANO, JORGELINA C.; FONTANA, ARIEL; WUILLOUD, RODOLFO G.

Kyoto

Simposio; 5th INTERNATIONAL SYMPOSIUM ON BROMINATED FLAME RETARDANTS; 2010

Kyoto University

PBDEs are one of the brominated flame retardants used to protect potentially flammable materials by increasing the resistance to ignition and delaying the spread of fire. PBDEs are additives of polymeric material and, thus are not chemically bound to the chemical structure. Therefore, they may leach from the surface of their product into the environment. PBDEs are persistent, have low water solubility and high affinity to suspended particles, which favors their bioaccumulation in hydrophobic mediums of the biota such as sediments. Sediment is one of the major sink to PBDEs in the aquatic environment. Since contaminants can be bioavailable in sediment to different aquatic organisms, the study of sediment is an important stage in tracing possible exposure route to aquatic biota. The purpose of the present work is to develop a new analytical methodology based on DSPE-DLLME, and demonstrate its applicability for extraction and preconcentration of PBDEs from sediment samples prior their determination by GC-MS/MS. To this aim, four of the most commonly found PBDEs in sediment samples were selected as target analytes: 2,2',4,4'- tetrabromodiphenyl ether (BDE-47), 2,2',4,4',5-pentabromodiphenyl ether (BDE-99), 2,2',4,4',6-pentabromodiphenyl ether (BDE-100), 2,2',4,4',5,5'-hexabromodiphenyl ether (BDE-153). The influence of several variables on the performance of the analytical methodology were studied and optimized over the analytical response of the PBDEs. The analytical performance of DSPE-DLLME-GC-MS/MS methodology was evaluated in terms of method detection limits (MDLs), repeatability and linear working range.