INVESTIGADORES
SILVA Maria Fernanda
artículos
Título:
Determination of polybrominated diphenyl ethers in water and soil samples by
Autor/es:
FONTANA, ARIEL R.; SILVA, MAR¡§ªA FERNANDA; MARTINEZ, LUIS DANTE; WUILLOUD, RODOLFO G.; ALTAMIRANO, JORGELINA C
Revista:
JOURNAL OF CHROMATOGRAPHY - A
Editorial:
Elsevier
Referencias:
Año: 2009 vol. 1216 p. 4339 - 4346
ISSN:
0021-9673
Resumen:
novel and efficient analytical methodology is proposed for extracting and preconcentrating polybrominated
diphenyl ethers (PBDEs) from samples of environmental interest prior gas chromatography¨Cmass
spectrometry (GC¨CMS) analysis. It is based on the induction of micellar organized medium by using a
non-ionic surfactant (Triton X-114) to extract the target PBDEs. To enable coupling the efficient extracting
technique with GC analysis, ultrasound-assisted back-extraction (UABE) into an organic solvent was
required. Several factors, including surfactant type and concentration, equilibration temperature and
time, ionic strength,pHand buffers nature and concentrationwere studied and optimized over the extraction
efficiency of the proposed technique. Under optimal experimental conditions, the target analytes
were quantitatively extracted achieving an enrichment factor of 250 when 10mL aliquot of ultrapure
water spiked with PBDE-standard mixture (10 pgmL−1 each PBDE) was extracted. Method detection
limits (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 ¡Ü8.5% (n = 5). The coefficients of estimation of the calibration
curves obtained following the proposedmethodologywere¡Ý0.9987 and linear range of all PBDEswas
4¨C150 pgmL−1. The proposedmethodologywas validated by carrying out a recovery study by spiking the
samples at two different concentration levels of PBDEs (10 and 50 pgmL−1 forwaters samples). Recoveries
values in the range of 96¨C106% for water samples were obtained showing satisfactory robustness of the
method for analyzing PBDEs in water samples. The proposed methodology was applied for the analysis
of PBDEs: 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) in water samples, including drinking, lake, river water and soil samples.
Significant quantities of PBDEs were not found in the analyzed samples.−1 each PBDE) was extracted. Method detection
limits (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 ¡Ü8.5% (n = 5). The coefficients of estimation of the calibration
curves obtained following the proposedmethodologywere¡Ý0.9987 and linear range of all PBDEswas
4¨C150 pgmL−1. The proposedmethodologywas validated by carrying out a recovery study by spiking the
samples at two different concentration levels of PBDEs (10 and 50 pgmL−1 forwaters samples). Recoveries
values in the range of 96¨C106% for water samples were obtained showing satisfactory robustness of the
method for analyzing PBDEs in water samples. The proposed methodology was applied for the analysis
of PBDEs: 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) in water samples, including drinking, lake, river water and soil samples.
Significant quantities of PBDEs were not found in the analyzed samples.−1 with RSDs values ¡Ü8.5% (n = 5). The coefficients of estimation of the calibration
curves obtained following the proposedmethodologywere¡Ý0.9987 and linear range of all PBDEswas
4¨C150 pgmL−1. The proposedmethodologywas validated by carrying out a recovery study by spiking the
samples at two different concentration levels of PBDEs (10 and 50 pgmL−1 forwaters samples). Recoveries
values in the range of 96¨C106% for water samples were obtained showing satisfactory robustness of the
method for analyzing PBDEs in water samples. The proposed methodology was applied for the analysis
of PBDEs: 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) in water samples, including drinking, lake, river water and soil samples.
Significant quantities of PBDEs were not found in the analyzed samples.¡Ý0.9987 and linear range of all PBDEswas
4¨C150 pgmL−1. The proposedmethodologywas validated by carrying out a recovery study by spiking the
samples at two different concentration levels of PBDEs (10 and 50 pgmL−1 forwaters samples). Recoveries
values in the range of 96¨C106% for water samples were obtained showing satisfactory robustness of the
method for analyzing PBDEs in water samples. The proposed methodology was applied for the analysis
of PBDEs: 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) in water samples, including drinking, lake, river water and soil samples.
Significant quantities of PBDEs were not found in the analyzed samples.−1. The proposedmethodologywas validated by carrying out a recovery study by spiking the
samples at two different concentration levels of PBDEs (10 and 50 pgmL−1 forwaters samples). Recoveries
values in the range of 96¨C106% for water samples were obtained showing satisfactory robustness of the
method for analyzing PBDEs in water samples. The proposed methodology was applied for the analysis
of PBDEs: 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) in water samples, including drinking, lake, river water and soil samples.
Significant quantities of PBDEs were not found in the analyzed samples.−1 forwaters samples). Recoveries
values in the range of 96¨C106% for water samples were obtained showing satisfactory robustness of the
method for analyzing PBDEs in water samples. The proposed methodology was applied for the analysis
of PBDEs: 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) in water samples, including drinking, lake, river water and soil samples.
Significant quantities of PBDEs were not found in the analyzed samples.