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通过凝聚萃取和液相色谱-荧光法测定废水和河水中的双酚A、双酚F及其二缩水甘油醚

Determination of bisphenols A and F and their diglycidyl ethers in wastewater and river water by coacervative extraction and liquid chromatography-fluorimetry.

作者信息

Ballesteros-Gómez Ana, Ruiz Francisco-Javier, Rubio Soledad, Pérez-Bendito Dolores

机构信息

Department of Analytical Chemistry, Facultad de Ciencias, Edificio Anexo Marie Curie, Campus de Rabanales 14071-Córdoba, Spain.

出版信息

Anal Chim Acta. 2007 Nov 5;603(1):51-9. doi: 10.1016/j.aca.2007.09.048. Epub 2007 Sep 29.

Abstract

A simple, rapid and sensitive analytical method was developed for the simultaneous determination of bisphenol A (BPA), bisphenol F (BPF) and their corresponding diglycidyl ethers (BADGE and BFDGE) in wastewater and river water, in order to have a useful tool for evaluating their fate and distribution in aquatic environments. It was based on their extraction with coacervates made up of decanoic acid reverse micelles and subsequent determination by liquid chromatography-fluorimetry. The procedure involved the extraction of 10.8 mL of water sample for 5 min, its centrifugation for 10 min to accelerate phase separation and then the chromatographic analysis of the target compounds. Clean-up or solvent evaporation steps were not necessary to get the required sensitivity and selectivity. Extraction efficiencies and concentration factors mainly depended on the amount of decanoic acid and tetrahydrofuran making up the coacervate. A general equation for the prediction of the volume of the coacervate as a function of its components has been proposed and fitted by nonlinear regression. This equation permits to know a priori the maximum concentration factors that can be achieved under given experimental conditions. Extractions were independent of salt addition (up to 1 M), the temperature (up to 60 degrees C) and the pH (below 4) rendering the method robust. Recoveries in samples ranged between about 80 and 92% and the actual concentrations factors were between 87 and 102, which resulted in practical detection limits around 30-35 ng L(-1). The method was successfully applied to the determination of the target pollutants in raw and treated sewage from four mechanical-biological treatment plants and three rivers. Bisphenols and their diglycidyl ethers were present in wastewater influents at concentrations in the range 0.96 to 1.6 microg L(-1). The biological treatment at the wastewater treatment plants (WWTP(s)) studied reduced the concentration of BPA and BPF in a percentage above 75%, while diglycidyl ethers were not detected in most of the effluents investigated. Only BPA was detected in surface waters.

摘要

开发了一种简单、快速且灵敏的分析方法,用于同时测定废水和河水中的双酚A(BPA)、双酚F(BPF)及其相应的二缩水甘油醚(BADGE和BFDGE),以便拥有一个评估它们在水生环境中归宿和分布的有用工具。该方法基于用由癸酸反胶束组成的凝聚层对其进行萃取,随后通过液相色谱 - 荧光法进行测定。该程序包括萃取10.8 mL水样5分钟,离心10分钟以加速相分离,然后对目标化合物进行色谱分析。为获得所需的灵敏度和选择性,无需进行净化或溶剂蒸发步骤。萃取效率和浓缩因子主要取决于构成凝聚层的癸酸和四氢呋喃的量。提出了一个预测凝聚层体积与其成分函数关系的通用方程,并通过非线性回归进行拟合。该方程允许事先了解在给定实验条件下可实现的最大浓缩因子。萃取不受加盐量(高达1 M)、温度(高达60摄氏度)和pH值(低于4)的影响,使该方法具有稳健性。样品中的回收率在约80%至92%之间,实际浓缩因子在87至102之间,实际检测限约为30 - 35 ng L⁻¹。该方法成功应用于四个机械 - 生物处理厂和三条河流的原污水和处理后污水中目标污染物的测定。双酚及其二缩水甘油醚在废水进水口的浓度范围为0.96至1.6 μg L⁻¹。所研究的污水处理厂(WWTP(s))的生物处理使BPA和BPF的浓度降低了75%以上,而在所调查的大多数流出物中未检测到二缩水甘油醚。仅在地表水中检测到了BPA。

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