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1.
J Chromatogr A ; 1192(1): 1-8, 2008 May 23.
Artículo en Inglés | MEDLINE | ID: mdl-18394632

RESUMEN

In this study, a method was developed for determination of steroid hormones (17beta-estradiol, estrone, 17alpha-ethynylestradiol) in tap and sewage water samples from Sweden. Sample preparation and analysis were performed by a hollow-fibre microporous membrane liquid-liquid extraction (HF-MMLLE) set-up combined with gas chromatography-mass spectrometry (GC-MS). In this approach, only the organic liquid in the lumen (10microL) of the hollow-fibre membrane was utilised for depleting extraction. Several parameters were studied, including: type of organic solvent, sample pH, salt and humic acid content. The optimised method allowed the determination of the analyte at the low ngL(-1) level in tap and sewage water. A linear plot gave correlation coefficients better than 0.995 and resulted in a method limit of detection of 1.6, 3 and 10ngL(-1) for 17beta-estradiol, estrone, and 17alpha-ethynylestradiol, respectively, in sewage water. Enrichment factors were over 1400 after derivatisation. The repeatabilities at 50 and 600ngL(-1) were better than 10% and 6%, respectively.


Asunto(s)
Estradiol/análisis , Estrona/análisis , Etinilestradiol/análisis , Cromatografía de Gases y Espectrometría de Masas/métodos , Hormonas Esteroides Gonadales/análisis , Contaminantes Químicos del Agua/análisis , Fraccionamiento Químico/métodos , Reproducibilidad de los Resultados , Aguas del Alcantarillado/química
2.
Chemosphere ; 63(9): 1532-8, 2006 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-16289218

RESUMEN

If the release mechanisms during selective chemical extraction of persistent organic pollutants (POP) mimic release mechanisms in natural systems during biological uptake, then a selective non-exhaustive extraction could give a quantitative measure of the bioavailable POP fraction. Supercritical fluid extraction (SFE) is suggested as a possible technique to estimate the amount of bioavailable polychlorinated biphenyls (PCBs) at contaminated sites and hence serve as a new tool in risk assessment. The uptake of PCBs by earthworm (Eisenia foetida) was investigated. PCB contaminated soil was pre-extracted with selective non-exhaustive SFE (50 degrees C, 350 bar, 1h), which removed on average 70% of the individual PCBs. Earthworms were placed in this pre-extracted soil, as well as in untreated soil. After 10 days, the PCB uptake by earthworms in the two systems was compared. The bioaccumulation factor (BAF) was 83% lower in the pre-extracted system than in the untreated system, demonstrating that SFE extracts primarily bioavailable contaminants. From the data, the bioavailable fraction could also be calculated to be 75%, which is very close to the 70% removed by SFE under the applied conditions. This suggests that the chemical methodology is capable of measuring the bioavailable fraction very accurately in this system.


Asunto(s)
Técnicas de Química Analítica/métodos , Oligoquetos/metabolismo , Bifenilos Policlorados/farmacocinética , Contaminantes del Suelo/farmacocinética , Animales , Disponibilidad Biológica , Bifenilos Policlorados/análisis , Contaminantes del Suelo/análisis
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