Department of Analytical Chemistry, University of Almeria, Spain.
Anal Chim Acta. 2011 May 5;693(1-2):62-71. doi: 10.1016/j.aca.2011.03.010. Epub 2011 Mar 9.
The objective of this study was the optimization and comparison of two extraction methods for the determination of polycyclic aromatic hydrocarbons (PAHs) in wastewater (WW). A distribution study of the target compounds between the aqueous phase and the suspended particulate matter (SPM) has been performed in order to establish whether the analysis of both phases is necessary. In this sense, the feasibility of stir bar sorptive extraction (SBSE) and solid-phase extraction (SPE) for the determination of 24 PAHs in WW samples has been evaluated. The results demonstrated the suitability of SBSE to perform a comprehensive analysis of liquid samples containing high amounts of SPM, such as in the determination of PAHs in WWs. A gas chromatography triple quadrupole mass spectrometry (GC-QqQ-MS/MS) method has been also optimized for the separation and detection of the target compounds, avoiding the co-elution of some groups of isomers, such as benzo[b], [j] and [k] fluoranthenes and indene[1,2,3-cd]pyrene/dibenz[a,h]anthracene. For that purpose, a specific capillary column developed for PAH determination was used. The SBSE procedure was validated and adequate parameters (such as recovery, linearity, precision, limits of detection and quantification) were obtained. Finally, the validated method was applied to the analysis of real samples collected from an experimental WW treatment plant, detecting some PAHs at concentrations in the range 0.007-0.022 μg L(-1).
本研究的目的是优化和比较两种提取方法，以测定废水中的多环芳烃（PAHs）。为了确定是否需要分析两个相，已经对目标化合物在水相和悬浮颗粒物（SPM）之间的分布进行了研究。在这个意义上，评估了搅拌棒吸附萃取（SBSE）和固相萃取（SPE）用于测定 WW 样品中 24 种 PAHs 的可行性。结果表明，SBSE 适用于对含有大量 SPM 的液体样品进行综合分析，例如 WW 中 PAHs 的测定。还优化了一种气相色谱三重四极杆质谱（GC-QqQ-MS/MS）方法，用于分离和检测目标化合物，避免了某些同系物组（如苯并[b]，[j]和[k]荧蒽和茚并[1,2,3-cd]芘/二苯并[a,h]蒽）的共洗脱。为此，使用了专门为 PAH 测定开发的毛细管柱。验证了 SBSE 程序，并获得了适当的参数（如回收率、线性度、精密度、检测限和定量限）。最后，将经过验证的方法应用于从实验性 WW 处理厂采集的实际样品的分析，检测到一些 PAHs 的浓度在 0.007-0.022 μg L（-1）范围内。
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