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The aim of this study was to develop and validate an analytical method for determining estrone, 17β-estradiol, 17α-ethynyl estradiol and diclofenac in whole surface water samples at or below the limits of quantification as set out in Decision 2015/495/EU. The method is based on solid-phase extraction using Atlantic® HLB disks in a semi-automated system (SPE-DEX® 4790). The method involved extracting 10L of whole surface water samples followed by derivatization with N-methyl-N-(trimethylsilyl)trifluoroacetamide) and analysis by gas chromatography-mass spectrometry. Drying the disks overnight at 25°C followed by elution with ethyl acetate resulted in extraction recoveries between 75.9% and 120% and limits of quantification of 0.290ngL(-1) for estrone, 1.37ngL(-1) for 17β-estradiol, 0.724ngL(-1) for 17α-ethynyl estradiol and 0.119ngL(-1) for diclofenac. Despite extracting 10L of sample, obtained limits of quantification for 17β-estradiol and 17α-ethynyl estradiol were above those set in the Decision 2015/495/EU, while limits of quantification for estrone and diclofenac were lower. The method was applied to six Slovene surface waters, among which four contained detectable concentrations of only diclofenac (0.313ngL(-1)-5.69ngL(-1)). To our knowledge, this is the first study reporting a large volume solid-phase extraction using disks for the determination of estrone, 17β-estradiol, 17α-ethynyl estradiol and diclofenac in whole surface waters.
This article was published in the following journal.
Name: The Science of the total environment
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An extraction method that separates analytes using a solid phase and a liquid phase. It is used for preparative sample cleanup before analysis by CHROMATOGRAPHY and other analytical methods.
Use of various chemical separation and extraction methods, such as SOLID PHASE EXTRACTION; CHROMATOGRAPHY; and SUPERCRITICAL FLUID EXTRACTION; to prepare samples for analytical measurement of components.
Fractionation of a vaporized sample as a consequence of partition between a mobile gaseous phase and a stationary phase held in a column. Two types are gas-solid chromatography, where the fixed phase is a solid, and gas-liquid, in which the stationary phase is a nonvolatile liquid supported on an inert solid matrix.
Colloids with a solid continuous phase and liquid as the dispersed phase; gels may be unstable when, due to temperature or other cause, the solid phase liquefies; the resulting colloid is called a sol.
Techniques used to separate mixtures of substances based on differences in the relative affinities of the substances for mobile and stationary phases. A mobile phase (fluid or gas) passes through a column containing a stationary phase of porous solid or liquid coated on a solid support. Usage is both analytical for small amounts and preparative for bulk amounts.