Simplified determination of lipophilic metabolites of nonylphenol ethoxylates: method development and application in aqueous samples from Buenos Aires, Argentina.
Simplified determination of lipophilic metabolites of nonylphenol ethoxylates: method development and application in aqueous samples from Buenos Aires, Argentina.
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DOI：
10.1039/b717942a
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发表时间：
2008-04
期刊：
影响因子：
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通讯作者：
P. Babay;Emiliano E Romero Ale;Raúl F. Itria;Elena T. Becquart;B. Thiele;D. Batistoni
中科院分区：
文献类型：
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作者：
P. Babay;Emiliano E Romero Ale;Raúl F. Itria;Elena T. Becquart;B. Thiele;D. Batistoni
在目前的工作中，我们已经开发了一种分析方法测定壬基酚（NP）和壬基酚单和二乙氧基化物（NP 1 EO和NP 2 EO）在水样中。通过对布宜诺斯艾利斯与环境有关的水样进行分析，证明了这种方法的适用性。这构成了对阿根廷NPnEO表面活性剂发生率进行严格评估的起点，因为到目前为止，关于这些化合物在当地系统中发生率的定性或半定量数据非常少。富集的分析物进行固相萃取的C-18吸附剂，然后用乙酸乙酯洗脱。正相高效液相色谱氨基硅胶柱和荧光检测器在230-300 nm的激发-发射波长用于分离和定量的分析物。通过离线耦合HPLC和GC-MS分析，确认所选真实的样品中的峰归属。使用非极性GC毛细管柱，并且获得每个乙氧基化同系物和NP的烷基链异构体的特征峰图案。在所有情况下，GC-MS分析得到HPLC收集的级分的纯度水平高于80%。发现NPnEO的雌激素代谢物浓度升高，这与该国不受限制地使用这类非离子表面活性剂是一致的。
In the present work we have developed an analytical methodology for the determination of nonylphenol (NP) and nonylphenol mono- and di-ethoxylates (NP1EO and NP2EO) in water samples. The applicability of this methodology was proved by means of the analysis of environmentally relevant aqueous samples from Buenos Aires. This constitutes a starting point for a rigorous assessment of the incidence of NPnEO surfactants in Argentina, as only very few, qualitative or semi-quantitative data on the occurrence of these compounds in local systems were available up to this time. Enrichment of the analytes was carried out by solid-phase extraction on a C-18 sorbent, followed by elution with ethyl acetate. Normal-phase high performance liquid chromatography on an amino-silica column and fluorescence detection at excitation-emission wavelengths of 230-300 nm were employed for separation and quantification of the analytes. Confirmation of peak assignment in selected real samples was performed by off-line coupling HPLC with GC-MS analysis. A non-polar GC capillary column was used, and a characteristic peak pattern was obtained for the alkyl chain isomers of each ethoxylated homologue and NP. GC-MS analyses yielded in all cases purity levels higher than 80% for the HPLC collected fractions. The elevated concentrations found for the estrogenic metabolites of NPnEO are in accordance with an unrestricted use of this class of non-ionic surfactants in the country.