Determination of polycyclic aromatic hydrocarbons and polycylic aromatic sulfur heterocycles by high-performance liquid chromatography with fluorescence and atmospheric pressure chemical ionization mass spectrometry detection in seawater and sediment samples

J Chromatogr A. 2002 Jun 7;958(1-2):141-8. doi: 10.1016/s0021-9673(02)00386-2.


Two methods for determining 10 polycyclic aromatic compounds were developed. Both methods were based on high-performance liquid chromatography (HPLC), but one method used fluorescence detection, while the other used atmospheric pressure chemical ionization mass spectrometry (APCI-MS). For water analysis, solid-phase extraction (SPE) was on-line coupled to the separation system. Using a styrene-divinylbenzene copolymer (PLRP-s) as sorbent in the SPE and adding 20% of acetonitrile to the water sample before its preconcentration, recoveries were above 70% for most of the compounds. For the fluorescence method, all compounds were detected and six of them could be quantified at concentrations higher than 0.02 microg 1(-1). For the MS detection method, only seven of the compounds were detected and six were quantified at concentrations higher than 0.06 microg 1(-1). To analyse sediment samples, an extraction with dichloromethane was used and, due to the complexity of the matrix, a standard addition calibration was carried out. Seawater and sediment samples taken from the Tarragona fishing port and marina on the coast of Catalonia (Spain) were analysed, and five compounds (benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, benzo[ghi]perylene and indeno[1,2,3-cd]pyrene) were quantified in the sediment samples.

MeSH terms

  • Atmospheric Pressure
  • Chromatography, High Pressure Liquid / methods*
  • Geologic Sediments / chemistry*
  • Heterocyclic Compounds / analysis*
  • Mass Spectrometry / methods*
  • Polycyclic Compounds / analysis*
  • Reference Standards
  • Seawater / chemistry*
  • Sensitivity and Specificity
  • Spectrometry, Fluorescence
  • Sulfur Compounds / analysis*


  • Heterocyclic Compounds
  • Polycyclic Compounds
  • Sulfur Compounds