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Determination of steroidal oestrogens in tap water samples using solid-phase extraction on a molecularly imprinted polymer sorbent and quantification with gas chromatography-mass spectrometry (GC-MS)

机译:使用分子印迹聚合物吸附剂上的固相萃取并通过气相色谱-质谱法(GC-MS)进行定量测定自来水样品中的甾体雌激素

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摘要

An analytical method was established and validated for the analysis of steroidal oestrogens in tap water samples. Gas chromatography coupled to high-resolution mass spectrometry (GC-HRMS) and gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) were used for the identification/quantification of selected compounds and the analytical performance of these techniques was evaluated. Liquid-liquid extraction (LLE) and solid-phase extraction (SPE) with a molecularly imprinted polymer (MIP) stationary phase that was highly selective for oestrogens were used for the extraction of 100-mL aliquots of water samples. The recoveries of analytes with the described methods ranged from 92 to 114 %, while the repeatability in terms of relative standard deviations (RSDs) was in the range from 2.1 to 15.2%(n = 5). It was concluded that SPE with MIP that was highly selective for oestrogens in combination with GC-HRMS detection is more preferable for the analysis of oestrogens in tap water samples. The typical oestrogen, 17 beta-estradiol (17 beta-E2), was detected above the method limit of quantification (m-LOQ) in 5 of 14 analysed tap water samples at concentrations from 0.09 to 0.15 ng L-1. Despite that 17 alpha-ethynylestradiol (17 alpha-EE2) was not quantified in this study above m-LOQ, the presence of this chemical was qualitatively confirmed in some of the analysed samples.
机译:建立了一种分析方法,并验证了该方法可用于分析自来水样品中的类固醇雌激素。气相色谱-高分辨质谱法(GC-HRMS)和气相色谱-串联质谱(GC-MS / MS)用于鉴定/量化所选化合物,并评估了这些技术的分析性能。对雌激素具有高选择性的分子印迹聚合物(MIP)固定相的液-液萃取(LLE)和固相萃取(SPE)用于萃取100 mL等份的水样。所描述方法的分析物回收率介于92%至114%之间,而相对标准偏差(RSD)的可重复性则介于2.1%至15.2%(n = 5)之间。结论是,结合MIP的SPE对雌激素具有高度选择性,结合GC-HRMS检测对于自来水样品中的雌激素分析更为优选。在0.09至0.15 ng L-1的浓度下,在14个分析的自来水样品中的5个中,检测到典型的雌激素17β-雌二醇(17 beta-E2)高于方法极限(m-LOQ)。尽管在这项研究中未在m-LOQ之上对17α-乙炔基雌二醇(17 alpha-EE2)进行定量,但在一些分析样品中定性地证实了该化学物质的存在。

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