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一种快速 UHPLC-MS/MS 法测定植物雌激素的方法及其在阿拉巴马河口的分布。

A rapid UHPLC-MS/MS method for quantitation of phytoestrogens and the distribution of enterolactone in an Alabama estuary.

机构信息

Department of Civil Engineering, Auburn University, Auburn, AL, 36849, USA.

Department of Civil Engineering, Auburn University, Auburn, AL, 36849, USA.

出版信息

Chemosphere. 2019 Dec;237:124472. doi: 10.1016/j.chemosphere.2019.124472. Epub 2019 Jul 27.

DOI:10.1016/j.chemosphere.2019.124472
PMID:31394445
Abstract

Endocrine disrupting chemicals (EDCs) are natural or synthetic compounds that can interfere with the endocrine systems of humans and wildlife. EDCs can pass through wastewater treatment systems, or run off from urban areas or agricultural operations, into natural water bodies, exposing resident and migratory organisms to complex EDC mixtures. Some phytoestrogenic polyphenolics (PEPP) are known or suspected EDCs; however, their contribution to total EDC burden in natural surface water systems is largely unknown. We describe a rapid, sensitive, and reproducible quantitative method for analysis of 15 PEPP in estuarine sediment and water, using ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UHPLC-MS/MS). The method provides excellent peak resolution, peak separation, and rapid run times (method separation/total run time: 8/12.5 min). With two exceptions, spiking experiments demonstrated that the percent recoveries for target PEPP in sediment and water samples were within acceptable analytical validation limits. LOD and LOQ values ranged from 0.004 to 0.010 ng/injection and 0.013-0.032 ng/injection, respectively. The validated method was used for PEPP analysis of sediment and water samples collected from 11 locations within the Perdido Bay estuary in coastal Alabama. No PEPP above the LOD were detected in sediment samples. The mammalian-derived lignin enterolactone was observed at low concentrations in water throughout the estuary, and significantly, at elevated concentrations at two locations associated with small-scale septic systems (3.66 ± 0.27 ng L and 4.01 ± 0.33 ng L) and a large wastewater treatment system (4.56 ± 0.24 ng L and 5.69 ± 0.43 ng L).

摘要

内分泌干扰化学物质(EDCs)是天然或合成的化合物,它们可以干扰人类和野生动物的内分泌系统。EDCs 可以通过废水处理系统,或者从城市地区或农业作业中流出,进入自然水体,使当地和洄游生物暴露于复杂的 EDC 混合物中。一些植物雌激素多酚(PEPP)是已知或疑似的 EDC;然而,它们对自然地表水系统中总 EDC 负担的贡献在很大程度上尚不清楚。我们描述了一种快速、灵敏和可重现的定量方法,用于分析河口沉积物和水中的 15 种 PEPP,使用超高效液相色谱-三重四极杆质谱联用(UHPLC-MS/MS)。该方法提供了极好的峰分辨率、峰分离和快速运行时间(方法分离/总运行时间:8/12.5 分钟)。除了两个例外,加标实验表明,目标 PEPP 在沉积物和水样中的回收率在可接受的分析验证限制内。LOD 和 LOQ 值范围分别为 0.004-0.010 ng/进样和 0.013-0.032 ng/进样。经过验证的方法用于分析阿拉巴马州沿海佩尔迪多湾河口 11 个地点采集的沉积物和水样中的 PEPP。在沉积物样品中未检测到高于 LOD 的 PEPP。哺乳动物衍生的木质素肠内酯在整个河口的水中均以低浓度存在,并且在与小型化粪池系统(3.66±0.27ng/L 和 4.01±0.33ng/L)和大型废水处理系统(4.56±0.24ng/L 和 5.69±0.43ng/L)相关的两个位置处浓度显著升高。

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