Chemical Faculty, Department of Chemical and Process Engineering, Gdansk University of Technology, Narutowicza St. 11/12, 80-233 Gdansk, Poland.
Anal Bioanal Chem. 2011 Aug;401(3):1059-69. doi: 10.1007/s00216-011-5134-9. Epub 2011 Jun 7.
This paper describes a novel method of sample preparation for the determination of trace concentrations of polycyclic aromatic hydrocarbons (PAHs) in high-boiling petroleum products. Limits of quantitation of the investigated PAHs in materials of this type range from tens of nanograms per kilogram to <20 μg/kg. The studies revealed that in order to separate most of interferences from the analytes without a significant loss of PAHs, it is necessary to use size exclusion chromatography as the first step of sample preparation, followed by adsorption using normal-phase liquid chromatography. The use of orthogonal separation procedure described in the paper allows the isolation of only a group of unsubstituted and substituted aromatic hydrocarbons with a specific range of molar mass. The lower the required limit of quantitation of PAHs, the larger is the scale of preparative liquid chromatography in both steps of sample preparation needed. The use of internal standard allows quantitative results to be corrected for the degree of recovery of PAHs during the sample preparation step. Final determination can be carried out using HPLC-FLD, GC-MS, or HPLC-UV-VIS/DAD. The last technique provides a degree of identification through the acquired UV-VIS spectra.
本文介绍了一种用于测定高沸点石油产品中痕量多环芳烃（PAHs）的新型样品制备方法。在所研究的材料中，调查 PAHs 的定量限从数十纳克/千克到<20μg/kg 不等。研究表明，为了在不显著损失 PAHs 的情况下将大多数干扰物与分析物分离，有必要将尺寸排阻色谱法作为样品制备的第一步，然后使用正相液相色谱法进行吸附。本文中描述的正交分离程序的使用允许仅分离一组具有特定摩尔质量范围的未取代和取代芳烃。所需 PAHs 的定量限越低，在样品制备的两个步骤中所需的制备液相色谱的规模就越大。使用内标可以对样品制备过程中 PAHs 的回收率进行定量结果的校正。最终测定可使用 HPLC-FLD、GC-MS 或 HPLC-UV-VIS/DAD 进行。最后一种技术通过获得的 UV-VIS 光谱提供一定程度的鉴定。
