Department of Environmental Sciences, Jožef Stefan Institute, Jamova cesta 39, 1000 Ljubljana, Slovenia; Jožef Stefan International Postgraduate School, Jamova cesta 39, 1000 Ljubljana, Slovenia.
Department of Environmental Sciences, Jožef Stefan Institute, Jamova cesta 39, 1000 Ljubljana, Slovenia; Jožef Stefan International Postgraduate School, Jamova cesta 39, 1000 Ljubljana, Slovenia.
Sci Total Environ. 2017 Jul 15;590-591:832-837. doi: 10.1016/j.scitotenv.2017.02.222. Epub 2017 Mar 8.
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 for estrone, 1.37ngL for 17β-estradiol, 0.724ngL for 17α-ethynyl estradiol and 0.119ngL 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-5.69ngL). 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.
本研究旨在开发和验证一种分析方法，用于在低于欧盟 2015/495 号决定规定的定量限以下测定全地表水样品中的雌酮、17β-雌二醇、17α-乙炔基雌二醇和双氯芬酸。该方法基于固相萃取，使用大西洋®HLB 圆盘在半自动系统（SPE-DEX®4790）中进行。该方法包括提取 10L 全地表水样品，然后用 N-甲基-N-（三甲基硅基）三氟乙酰胺衍生化，并用气相色谱-质谱法分析。将圆盘在 25°C 下干燥过夜，然后用乙酸乙酯洗脱，得到的提取回收率在 75.9%至 120%之间，雌酮的定量限为 0.290ng/L，17β-雌二醇为 1.37ng/L，17α-乙炔基雌二醇为 0.724ng/L，双氯芬酸为 0.119ng/L。尽管提取了 10L 样品，但获得的 17β-雌二醇和 17α-乙炔基雌二醇的定量限高于欧盟 2015/495 号决定的规定，而雌酮和双氯芬酸的定量限较低。该方法应用于斯洛文尼亚的 6 个地表水，其中 4 个仅含有可检测浓度的双氯芬酸（0.313ng/L-5.69ng/L）。据我们所知，这是第一项使用圆盘测定全地表水样品中雌酮、17β-雌二醇、17α-乙炔基雌二醇和双氯芬酸的大容量固相萃取研究。
