Sanz-Landaluze J, Bartolome L, Zuloaga O, González L, Dietz C, Cámara C
Department of Analytical Chemistry, Faculty of Chemistry, University Complutense de Madrid, Ciudad Universitaria, 28040, Madrid, Spain.
Anal Bioanal Chem. 2006 Mar;384(6):1331-40. doi: 10.1007/s00216-005-0249-5. Epub 2006 Feb 25.
A rapid and simple method is proposed for determination of polycyclic aromatic hydrocarbons (PAH) in complex matrices such as marine biota. The method uses sonication, by means of an ultrasonic probe, as a new tool for assisted extraction, coupled with reversed-phase liquid chromatography (RP-LC) with fluorescence detection (FL) for determination of 16 US EPA priority PAH. Separation and detection of the 16 PAH were complete in 45 min by RP-LC with a C18 column and acetonitrile-water gradient elution. Multivariate optimisation of the variables affecting extraction (ultrasound radiation amplitude, sonication time, and temperature of the water-bath in which the extraction cell was placed) was conducted. The accuracy of the method was determined by analysis of a certified reference material and comparison of the results obtained with those from another method (microwave-assisted extraction and GC-MS). The new technique avoids the main problems encountered in the determination of PAH in complex matrices such as marine biota, and no clean-up step is necessary. The method was applied to determination of PAH in estuarine biota samples from the Urdaibai estuary (Biscay, Spain).
本文提出了一种快速简便的方法,用于测定海洋生物群等复杂基质中的多环芳烃(PAH)。该方法采用超声探头进行超声处理,作为辅助萃取的新工具,并结合反相液相色谱(RP-LC)和荧光检测(FL)来测定16种美国环保署优先控制的PAH。使用C18柱和乙腈-水梯度洗脱,通过RP-LC在45分钟内完成了16种PAH的分离和检测。对影响萃取的变量(超声辐射幅度、超声处理时间以及放置萃取池的水浴温度)进行了多变量优化。通过分析有证标准物质并将所得结果与另一种方法(微波辅助萃取和GC-MS)的结果进行比较,确定了该方法的准确性。这项新技术避免了在测定海洋生物群等复杂基质中的PAH时遇到的主要问题,无需净化步骤。该方法应用于西班牙比斯开湾乌尔代阿伊河口的河口生物群样本中PAH的测定。