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一种用于同时分析水和沉积物中酚类和甾体雌激素的改进方法。

An improved method for the simultaneous analysis of phenolic and steroidal estrogens in water and sediment.

作者信息

Hibberd A, Maskaoui K, Zhang Z, Zhou J L

机构信息

Department of Biology and Environmental Science, School of Life Sciences, University of Sussex, Falmer, Brighton, UK.

出版信息

Talanta. 2009 Feb 15;77(4):1315-21. doi: 10.1016/j.talanta.2008.09.006. Epub 2008 Sep 12.

Abstract

This paper describes an improved method for the extraction and analysis of seven endocrine disrupting chemicals with wide-ranging polarities from water and sediments using gas chromatography-tandem mass spectrometry (GC-MS/MS). The analytes were 4-tert-octylphenol, 4-nonylphenol, bisphenol A, estrone, 17beta-estradiol, 17alpha-ethynylestradiol and 16alpha-hydroxyestrone. The optimised GC-MS/MS method produces increased selectivity and sensitivity compared to GC-MS, with limit of detection ranging from 0.01 to 0.49 ng L(-1) in water and from 0.05 to 0.14 ng g(-1) in sediment. Extraction from aqueous samples was performed by solid-phase extraction (SPE) and from sediment samples by microwave-assisted extraction (MAE). The improved method for the clean-up of sediment extracts carried out by SPE enhanced EDC recovery (86-102%) while reducing matrix interference and sample drying time. Derivatisation of final sample extracts was achieved using N,O-bis(trimethylsilyl)trifluoroacetamide and pyridine, and their stability was enhanced by reconstituting the derivatised extracts with hexane. The method was validated by spiking experiments which showed good recovery and reproducibility. The method was applied to samples taken from the Medway estuary in Kent, UK, where non-conservative behaviour of EDCs was demonstrated.

摘要

本文介绍了一种改进的方法,用于使用气相色谱 - 串联质谱法(GC-MS/MS)从水和沉积物中提取和分析七种极性范围广泛的内分泌干扰化学物质。分析物为4-叔辛基苯酚、4-壬基苯酚、双酚A、雌酮、17β-雌二醇、17α-乙炔基雌二醇和16α-羟基雌酮。与GC-MS相比,优化后的GC-MS/MS方法具有更高的选择性和灵敏度,在水中的检测限为0.01至0.49 ng L(-1),在沉积物中的检测限为0.05至0.14 ng g(-1)。水样的提取采用固相萃取(SPE),沉积物样品的提取采用微波辅助萃取(MAE)。通过SPE对沉积物提取物进行净化的改进方法提高了内分泌干扰物的回收率(86 - 102%),同时减少了基质干扰和样品干燥时间。最终样品提取物的衍生化使用N,O-双(三甲基硅基)三氟乙酰胺和吡啶实现,通过用己烷重构衍生化提取物提高了其稳定性。该方法通过加标实验进行了验证,结果显示回收率和重现性良好。该方法应用于从英国肯特郡的梅德韦河口采集的样品,结果表明了内分泌干扰物的非保守行为。

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