A rapid method for determining phenolic endocrine disrupters in water samples

Chromatographia (Impact Factor: 1.37). 10/2002; 56(9):573-576. DOI: 10.1007/BF02497672

ABSTRACT We have developed a method based on solid-phase extraction coupled on-line to liquid chromatography with UV detection (SPE-HPLC-UV)
to determine bisphenol A and a group of alkylphenols, which have been recognized as endocrine disrupters (ED), in water samples.
We optimized the conditions used for both SPE and the chromatography. The SPE-HPLC-UV method developed is rapid and it enables
routine analysis. Its performance was checked with a variety of aqueous samples collected in the south of Catalonia from the
Ebro river, from the sea, and from tapwater-and waste-water-treatment plants. Drinking water in plastic bottles was also analyzed.
The method enabled determination of ED at low levels; the limits of detection were between 0.01 and 0.1 μg L−1. Bisphenol A and nonylphenol were dttected in some samples.

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    • "Most of them couple a pre-concentration technique, namely liquid–liquid extraction (LLE) and solid phase extraction (SPE) with gas chromatography (GC), with several types of detectors: flame ionisation detector (FID) (Almeida et al., 1996; US EPA Method 8041, 1996; European Standard, 1998; Barták et al., 2000) and electronic capture detector (ECD) (European Standard, 1998; Barták et al., 2000). There are also a significant number of publications about the determination of phenolic compounds by capillary electrophoresis (Morales and Cela, 1999; Jáuregyu et al., 2000; Morales and Cela, 2000) and by high-performance liquid chromatography (HPLC) (Zhao and Lee, 2001; Liu et al., 2003), using solid-phase extraction (SPE) (Rodrí guez et al., 2000; Brossa et al., 2002; Wissiak and Rosenberg, 2002) or solid-phase microextraction (SPME) (Gonzalez-Toledo et al., 2001; Peñ alver et al., 2002; Sarrion et al., 2002; Canosa et al., 2005), as a pre-concentration step. Some of these methods include a derivatization step, in order to improve the detection signal and the resolution between peaks, especially between isomers (Buchholz and Pawliszyn, 1994; Moeder et al., 2000; Llompart et al., 2002; Korenman et al., 2003). "
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    ABSTRACT: A procedure based on solid-phase microextraction (SPME) and gas chromatography coupled with mass spectrometry (GC-MS) was developed and validated in order to analyse 10 phenols in water samples. The optimised conditions were obtained using polyacrylate fibre (PA), 20ml of sample volume, 10% NaCl, pH 4.0 and direct extraction at 35 degrees C and 1000rpm, for 40min. The linear range and quantification limits for these compounds by SPME-GC-MS were defined. An evaluation of the main uncertainty sources of this method is included, which allows expanded uncertainties in the 9.4-35% range for the majority of the compounds. The main source of uncertainty is associated with matrix effects. The validated method is suitable for monitoring the production and distribution of potable water and was used, in field trials, for the analysis of samples from main intakes of water (surface or underground) and from water supply system of a large area (Lisbon and neighbour municipalities).
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    ABSTRACT: This paper presents a gas chromatography-mass spectrometry method for simultaneous detection of five selected phenolic xenoestrogens. These include 4,4-biphenyldiol (4,4-dihydroxybiphenyl), 3-hydroxybiphenyl (m-phenylphenol), and 6-bromo-2-naphthol. In each analysis, one liter of water sample was extracted by using solid phase extraction (SPE) method. A simple and yet reliable derivatization reagent (i.e. trimethylphenylammonium hydroxide solution) was used in this study to enhance detection sensitivity. The method detection limits of the proposed method for the selected phenolic xenoestrogens were found to fall within the range of 2.3 to 12.4 ng L–1. Results of recovery tests showed that recoveries of the selected phenolic xenoestrogens in deionized water were within the range of 64% to 88% with relative standard deviations of 4% to 17% (n=10), when spiked with 100 and 500 ng L–1 of standards. The corresponding results for the fortified treated wastewater samples were 69% to 87% and 5% to 12% (n=7), respectively. The proposed method was successfully applied for detecting the selected xenoestrogens in tap water, treated wastewater and fortified deionized water. It was noted that the target compounds, at low ng L–1 levels, could be detected in treated wastewater samples.
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    ABSTRACT: This paper is a review with more than 100 references discussing the immunochemical methods reported in the literature for the most important man-made chemicals with suspected endocrine disrupting activity. Details regarding immunizing hapten design, antibody production, and the features (limit of detection, dynamic range, specificity) of the most important immunochemical methods developed (ELISA, FIIA, immunosorbents, immunosensors, etc.) are presented for important environmental pollutants such as bisphenol A, phthalates, alkylphenol polyethoxylates, alkylphenols, polychlorinated biphenyl compounds, and dioxins. Availability of commercial reagents and methods is reported.
    Analytical and Bioanalytical Chemistry 03/2004; 378(3):563-75. DOI:10.1007/s00216-003-2228-z · 3.58 Impact Factor
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