Journal
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
Volume 401, Issue 3, Pages 1059-1069Publisher
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-011-5134-9
Keywords
Sample preparation techniques; Multidimensional liquid chromatography; Group separation; Size exclusion chromatography; Normal-phase adsorption chromatography; High-boiling petroleum products; Polycyclic aromatic hydrocarbons (PAHs); Trace analysis
Funding
- State Committee for Scientific Research, Warsaw, Poland [N N523 4531 33]
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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 mu g/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.
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