PubMed · 13608938
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W M ALLEN. 1958. Functional uterine bleeding.. https://doi.org/10.1097/00003081-195809000-00027
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Two GC-MS methods, based on the application of N,O-bis(trimethylsilyl)trifluoroacetamide-derivatization-GC-MS (selected-ion monitoring) and GC-MS-MS without derivatization, respectively, were optimised and applied to the determination of a group of five selected endocrine disrupting compounds (EDCs) in wastewaters. Both methods included solid-phase extraction with Oasis HLB cartridges allowing an enrichment factor for wastewater samples of 100-fold. The investigated EDCs were estrone, 17beta-estradiol, 17alpha-ethynylestradiol, 4-tert-octylphenol and bisphenol A. Results obtained from the validation studies yielded comparable results in both cases. Recoveries in spiked wastewaters at 50 ng/l were higher than 90% for all the compounds, except for 4-tert-octylphenol (75%). Repeatability and reproducibility were adequate, varying from 1.6 to 14%, except for estrone which reproducibility was 28% when the derivatization-GC-MS method was applied. Limits of detection calculated ranged from 2.5 to 27.5 ng/l with differences between both methods from 1.1 (estrone) to 10.4 (bisphenol A) times. Both methods were successfully applied to the analysis of the target compounds in sewage treatment plant influents and effluents. Traces of bisphenol A, 4-tert-octylphenol, estrone and 17beta-estradiol were detected at concentration levels ranging from 13.3 to 1105.2 ng/l.
In this study, microwave-assisted extraction (MAE) followed by gas chromatography (GC)-mass spectrometry (MS) analysis has been successfully developed for the simultaneous extraction and determination of contrasting endocrine disrupting chemicals (EDCs) including 17beta-estradiol, estrone, 17(alpha-ethynylestradiol, 16alpha-hydroxyestrone, 4-nonylphenol, 4-tert-octylphenol and bisphenol A in river sediments. For MAE, the effects of various parameters on the extraction efficiency were investigated. It is shown that the most efficient extraction (recovery > 74%) of the target compounds was achieved by using methanol as the solvent, an extraction temperature of 110 degrees C and 15 min of holding time. The cleanup of extracts was carried out by passage through a non-deactivated silica gel column, and a satisfactory elution efficiency of all compounds was achieved using a solvent mixture of ethyl acetate-hexane (4:6, v/v). The spiking experiments show that the mean recovery of the target compounds exceeded 61% at a spiking level of 5 ng/g dry mass, and 73% at 10, 40 and 100 ng/g dry mass with a good reproducibility. The method developed was applied to the determination of target EDCs in river sediments collected from rivers Uck and Ouse, UK, and results revealed the presence of the chosen compounds at low ng/g level.
A readily applicable method based on extraction by aqueous non-ionic surfactant solutions (Tween 80) and RP-HPLC coupled to fluorescence detection, has been developed for the simultaneous determination of the phenolic endocrine disrupting chemicals (EDCs) nonylphenol (NP), nonylphenol monoethoxylate (NP1EO) and nonylphenol diethoxylate (NP2EO) and bisphenol A (BPA) in environmental solid matrices. Clean up of sample extracts was performed on Si-C18 solid phase extraction (SPE) cartridges. The overall Tween 80 extraction-SPE-RP-HPLC procedure was validated for accuracy and precision by analyzing sediment samples spiked with known amounts of EDCs. Recoveries for NP, NP1EO, NP2EO and BPA and limits of detection are in agreement with conventional extraction methods. The developed methodology was successfully applied to the analysis of target compounds in Italian river sediments, river suspended matter and benthonic macroinvertebrate organisms (oligochaetes Lumbriculus variegatus). Results confirmed that this relatively simple procedure performed satisfactorily in the determination of phenolic EDCs in environmental solid matrices of different complexity and that it can be a suitable alternative method to conventional systems even for routine analyses.