Micellar Organized Medium as Extraction and Preconcentration Technique for GC-MS: Determination of Brominated Flame Retardants in Water Samples

FONTANA, A.; SILVA, M.F.; DE SOUZA DIAS, F. S.; WUILLOUD, R.; MARTINEZ, L.; ALTAMIRANO, J.

Florianópolis

Congreso; Latin American Congress of Chromatography and Related Techniques. COLACRO XII; 2008

Instituto Internacional de Cromatografía

A novel and efficient analytical methodology is proposed for extracting and preconcentrating polybrominated diphenyl ethers (PBDEs) from water samples prior gas chromatography-mass spectrometry (GC-MS) analysis. PBDEs are a group of environmental persistent pollutants, which are related to health risks such as endocrine disruption, adverse neurobehavioral effects and probable carcinogens. The proposed methodology is based on the induction of micellar organized mediums by using a non-ionic surfactant (Triton X-114) to extract the target PBDEs. Due to the high viscosity of the surfactant phase, it is not possible to inject it into the GC column; therefore an ultrasound back-extraction into an organic solvent (isooctane) was applied in order to enable the efficient coupling of the extracting technique with GC-analysis. Under optimum experimental conditions, the target analytes were quantitatively extracted achieving an enrichment factor of 200 when 10 mL of 10 pg mL-1 PBDEs mix was extracted. Detection limits calculated as three times the signal-to-noise ratio (S/N), ranged from 0.8 to 2 pg mL-1 and the RSD were lower than 7.2 % (n = 5) when 10 pg mL-1 PBDEs water solution was analyzed. Although significant quantities of PBDEs weren not found in the analyzed samples, recoveries values in the range of 96-106% were obtained showing a successful robustness of the method for analyzing PBDEs in water samples.