Determination of polybrominated diphenyl ethers in water and soil samples by cloud point extraction-ultrasound-assisted back-extraction-gas chromatography-mass spectrometry

FONTANA, A.R., ALTAMIRANO, J.C.; SILVA MARÍA F.; MARTINEZ, L. D; WUILLOUD, R.G.; ALTAMIRANO, J.C.

JOURNAL OF CHROMATOGRAPHY - A

Elsevier

Año: 2009 p. 4339 - 4346

0021-9673

A novel and efficient analytical methodology is proposed for extracting and preconcentrating polybrominateddiphenyl ethers (PBDEs) from samples of environmental interest prior gas chromatography–massspectrometry (GC–MS) analysis. It is based on the induction of micellar organized medium by using anon-ionic surfactant (Triton X-114) to extract the target PBDEs. To enable coupling the efficient extractingtechnique with GC analysis, ultrasound-assisted back-extraction (UABE) into an organic solvent wasrequired. Several factors, including surfactant type and concentration, equilibration temperature andtime, ionic strength,pHand buffers nature and concentrationwere studied and optimized over the extractionefficiency of the proposed technique. Under optimal experimental conditions, the target analyteswere quantitatively extracted achieving an enrichment factor of 250 when 10mL aliquot of ultrapurewater spiked with PBDE-standard mixture (10 pgmL−1 each PBDE) was extracted. Method detectionlimits (MDLs) calculated with aqueous PBDEs solutions as three times the signal-to-noise ratio (S/N),ranged from 1 to 2 pgmL−1 with RSDs values ≤8.5% (n = 5). The coefficients of estimation of the calibrationcurves obtained following the proposedmethodologywere≥0.9987 and linear range of all PBDEswas4–150 pgmL−1. The proposedmethodologywas validated by carrying out a recovery study by spiking thesamples at two different concentration levels of PBDEs (10 and 50 pgmL−1 forwaters samples). Recoveriesvalues in the range of 96–106% for water samples were obtained showing satisfactory robustness of themethod for analyzing PBDEs in water samples. The proposed methodology was applied for the analysisof PBDEs: 2,2,4,4-tetraBDE (BDE-47), 2,2,4,4,5-pentaBDE (BDE-99), 2,2,4,4,6-pentaBDE (BDE-100) and2,2,4,4,5,5-hexaBDE (BDE-153) in water samples, including drinking, lake, river water and soil samples.Significant quantities of PBDEs were not found in the analyzed samples.© 2009