Martinez Elena, Gros Meritxell, Lacorte Sílvia, Barceló Damià
Department of Environmental Chemistry, IIQAB-CSIC, Jordi Girona 18-26, 08034 Barcelona, Catalonia, Spain.
J Chromatogr A. 2004 Aug 27;1047(2):181-8.
We describe in this paper simple and robust analytical protocols to determine the 16 polycyclic aromatic hydrocarbons (PAHs) of the US Environmental Protection Agency priority list in water, sediment and mussels. For water samples, eight different solid-phase extraction (SPE) sorbents have been compared and among them, C18 provided highest recoveries and limits of detection of 0.3-15 ng/L. For lyophilized sediments, Soxhlet and ultrasonic extraction were compared, and the last one permitted to recover all analytes with highest repetitivity and was validated by analysing a certified reference material. Finally, the analysis of mussels was undertaken using Soxhlet, ultrasonic and pressurized liquid extraction (PLE) and the performance of several clean-up steps are compared. Whereas for the former two, incomplete recovery or losses of some analytes were evidenced, PLE permitted a more efficient extraction and although alkaline digestion was necessary to remove coextracted compounds, the method gave acceptable recoveries and limits of detection of 0.5-7.7 microg/kg dry mass, as for sediments. In all cases, analysis was performed by gas chromatography coupled to mass spectrometry and internal standard quantification was performed using five deuterated PAHs. Each method performance is discussed for the three matrices analysed and the paper reports advantages and disadvantages of each for their routine application in monitoring programs.
我们在本文中描述了简单且稳健的分析方法，用于测定美国环境保护局优先清单中的16种多环芳烃（PAHs）在水、沉积物和贻贝中的含量。对于水样，比较了八种不同的固相萃取（SPE）吸附剂，其中C18的回收率最高，检测限为0.3 - 15 ng/L。对于冻干沉积物，比较了索氏提取法和超声提取法，后者能够以最高的重复性回收所有分析物，并通过分析有证标准物质进行了验证。最后，使用索氏提取法、超声提取法和加压液体萃取（PLE）对贻贝进行分析，并比较了几种净化步骤的性能。对于前两种方法，发现一些分析物回收不完全或有损失，而PLE能实现更高效的萃取，尽管需要进行碱性消解以去除共萃取的化合物，但该方法的回收率和检测限与沉积物一样，分别为0.5 - 7.7 μg/kg干质量，是可接受的。在所有情况下，均通过气相色谱 - 质谱联用进行分析，并使用五种氘代PAHs进行内标定量。针对所分析的三种基质，讨论了每种方法的性能，本文还报告了每种方法在监测计划中的常规应用的优缺点。
