在进行生物分析评估前通过固相萃取富集废水中微污染物的指南

IF 6 3区 环境科学与生态学 Q1 ENVIRONMENTAL SCIENCES
Tobias Schulze, Peta A. Neale, Jörg Ahlheim, Liza-Marie Beckers, Maria König, Janet Krüger, Margit Petre, Aleksandra Piotrowska, Rita Schlichting, Susanne Schmidt, Martin Krauss, Beate I. Escher
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引用次数: 0

摘要

背景废水中可能含有复杂的有机微污染物混合物,需要采用化学分析和基于效应的方法来识别相关微污染物并检测混合物效应。固相萃取(SPE)通常用于在分析前富集微污染物。固相萃取法对单个微污染物的回收率和稳定性进行了深入研究,但很少有研究针对基于效应的方法对固相萃取法进行优化。本研究的目的是开发和评估两种富集微污染物的标准操作程序 (SOP),以便为化学分析和生物分析做准备,其中一种涵盖了广泛的化学物质,另一种则选择性地富集雌激素类化学物质。结果用添加了 > 600 种微污染物的地表水开发了一种通用萃取方法,用于富集具有广泛理化特性的微污染物;而用添加了雌激素类化学物质的水确定了一种选择性萃取方法。对三种不同的固相萃取吸附剂进行了测试,评估了各种化学物质的回收率以及在致突变性、雌激素活性和鱼胚胎毒性试验中的效果。选择 pH 值为 7 的吸附剂 HRX 作为通用萃取方法,因为该吸附剂在生物测定中对各种化学物质的回收率和效果都最好。pH 值为 3 的吸附剂 HLB 对雌激素化学物质和雌激素活性的回收率最佳。这两种最佳的固相萃取法适用于加标和未加标废水,检测到的化学物质浓度和观察到的效果与之前的研究结果相似。对使用 HRX 和 HLB 方法萃取后的提取物和固相萃取柱进行了雌激素和雌激素活性的长期储存评估,使用 HLB 方法 112 天后,雌激素的有效性接近 100%。不过,如果实验室只想使用一种固相萃取吸附剂,那么 HLB 既可用于一般萃取,也可用于选择性萃取,因为它对多种微污染物的化学回收率和效果与 HRX 相似。本文的最终 SOP 是对本文的补充,其中包括一个用于普通萃取的变体和一个用于萃取雌激素类化学物质的变体。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
A guidance for the enrichment of micropollutants from wastewater by solid-phase extraction before bioanalytical assessment

Background

Wastewater can contain a complex mixture of organic micropollutants, with both chemical analysis and effect-based methods needed to identify relevant micropollutants and detect mixture effects. Solid-phase extraction (SPE) is commonly used to enrich micropollutants prior to analysis. While the recovery and stability of individual micropollutants by SPE has been well studied, few studies have optimized SPE for effect-based methods. The aim of the current study was to develop and evaluate two standard operating procedures (SOPs) for the enrichment of micropollutants in preparation for chemical analysis and bioanalysis, one covering a broad range of chemicals and the other selective for estrogenic chemicals.

Results

Pristine surface water spiked with > 600 micropollutants was used to develop a generic extraction method for micropollutants with a wide range of physiochemical properties, while water spiked with estrogenic chemicals was used to identify a selective extraction method. Three different SPE sorbents were tested, with recoveries of individual chemicals and effect in assays indicative of mutagenicity, estrogenic activity, and fish embryo toxicity assessed. The sorbent HRX at pH 7 was selected for the generic extraction method as it showed the best recovery of both individual chemicals and effect in the bioassays. The sorbent HLB at pH 3 showed optimal recovery of estrogenic chemicals and estrogenic activity. The two optimal SPE methods were applied to spiked and unspiked wastewater effluents, with the concentrations of detected chemicals and observed effects similar to those of previous studies. The long-term storage of both extracts and SPE cartridges for estrogens and estrogenic activity after extraction with the HRX and HLB methods were evaluated, with estrogenic effectiveness close to 100% after 112 days when HLB was used.

Conclusions

HRX is recommended for generic extraction, while HLB is optimal for the selective extraction of estrogenic micropollutants. However, if a laboratory only wants to use a single SPE sorbent, HLB can be used for both generic and selective extraction as it yielded similar chemical and effect recovery as HRX for a wide range of micropollutants. This paper is supplemented by the final SOP that includes a variant for generic extraction and one for the extraction of estrogenic chemicals.

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来源期刊
Environmental Sciences Europe
Environmental Sciences Europe Environmental Science-Pollution
CiteScore
11.20
自引率
1.70%
发文量
110
审稿时长
13 weeks
期刊介绍: ESEU is an international journal, focusing primarily on Europe, with a broad scope covering all aspects of environmental sciences, including the main topic regulation. ESEU will discuss the entanglement between environmental sciences and regulation because, in recent years, there have been misunderstandings and even disagreement between stakeholders in these two areas. ESEU will help to improve the comprehension of issues between environmental sciences and regulation. ESEU will be an outlet from the German-speaking (DACH) countries to Europe and an inlet from Europe to the DACH countries regarding environmental sciences and regulation. Moreover, ESEU will facilitate the exchange of ideas and interaction between Europe and the DACH countries regarding environmental regulatory issues. Although Europe is at the center of ESEU, the journal will not exclude the rest of the world, because regulatory issues pertaining to environmental sciences can be fully seen only from a global perspective.
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