Progress of Cryogenics and Isotopes Separation , ISSN: 1582-2575
2019, Volume 22, Issue 2
Pages 43-54

Assessment of PAHs levels in sediments and fish collected from artificial lakes on the course of Olt river, Romania: Optimisation and validation of the extraction methods

Corina Teodora Ciucure , Elisabeta-Irina Geana *

National Research and Development Institute for Cryogenics and Isotopic Technologies - ICSI Rm. Valcea, Uzinei Street no. 4, PO Box Râureni 7, 240050, Râmnicu Vâlcea, Romania

*Corresponding author: Elisabeta-Irina Geana, E mail:

Received 20 September 2019
Received in revised form 15 October 2019
Accepted 17 October 2019
Available online 20 November 2019


In this work the procedures for the analysis of 15 prioritary PAHs in sediment and fish samples were optimised and validated. Different extraction protocoles: Energized Dispersive Extraction (EDGE) and ultrasonic solvent extraction procedures with hexane:acetone 1:1 and dichloromethane for sediments and solid-lichid extraction procedure combined with lipids hydrolysis with potassium hydroxide for fish, were used for PAHs isolation from sediments and fish material prior to HPLC-FL analysis. General analytical procedures were validated by systematic recovery experiments using sediment standard reference material ERM-CC013a and by spiking experiments at three levels in the case of fish.
The targeted priority PAHs, except naphthalene, acenaphthene and dibenz(a,h)anthracene, were successfully extracted from ERM-CC013a certified material, with recoveries ranging from 61.9-125.2 % with variation coefficients not exceeding 10%. Ultrasonic extraction procedure with dichloromethane during 30 min presented good analytical performances (recoveries ranging from 79.0% to 103.3%, precision within 10% for all the PAHs, quantification limits ranging from 0.05-0.94 μg/kg). In the case of fish matrix, the extraction procedure shows satisfactory recoveries, facilitating the determination of all PAHs regulated well below the value of the concentrations imposed today. Limits of quantification (LOQs) ranged between 0.065-0.675 μg/kg fresh fish.
The optimised procedures were applied to assess the level of 15 PAHs in the sediments and fish samples from artificial lackes on the middle and lower course of Olt river, Romania, during January and February 2019, in order to estimate the concentrations and possible origins of contamination and to assess the safety concerning PAHs contents of different fish species.


  • Abdel-Shafy, H. I., & Mansour, M. S. M. (2016)
    A review on polycyclic aromatic hydrocarbons: Source, environmental impact, effect on human health and remediation
    Egyptian Journal of Petroleum, 25, 107-123.

  • Baumard, P., Budzinski, H., & Garrigues, P. (1998)
    Polycyclic aromatic hydrocarbons in sediments and mussels of the western Mediterranean sea
    Environmental Toxicology and Chemistry, 17(5), 765-776.

  • Bogdanović, T., Pleadin, J., Petričević, S., Listeš, E., Sokolić, D., Marković, K., … Šimat, V. (2019)
    The occurrence of polycyclic aromatic hydrocarbons in fish and meat products of Croatia and dietary exposure
    Journal of Food Composition and Analysis, 75, 49-60.

  • Dong, C.-D., Chen, C.-F., Chen, C.-W., Dong, C.-D., Chen, C.-F., & Chen, C.-W. (2012)
    Determination of Polycyclic Aromatic Hydrocarbons in Industrial Harbor Sediments by GC-MS
    International Journal of Environmental Research and Public Health, 9(6), 2175-2188.

  • European Commission. (2007)
    REGULAMENTUL (CE) NR. 1881/2006 AL Comisiei din 19 decembrie 2006 de stabilire a nivelurilor maxime pentru anumiți contaminanți din produsele alimentare

  • Fischer, K., Fries, E., Körner, W., Schmalz, C., & Zwiener, C. (2012)
    New developments in the trace analysis of organic water pollutants
    Applied Microbiology and Biotechnology, 94(1), 11- 28.

  • Iordache, M., Iordache, A.M., Sandru, C, Voica, C., Zgavarogea, R., Miricioiu, M., Ionete, R.E. (2019)
    Assessment of Heavy Metals Pollution in Sediments from Reservoirs of the Olt River as Tool for Environmental Risk Management
    Rev. Chim. (Bucharest)

  • Peng, X., Jin, J., Wang, C., Ou, W., & Tang, C. (2015)
    Multi-target determination of organic ultraviolet absorbents in organism tissues by ultrasonic assisted extraction and ultra-high performance liquid chromatography–tandem mass spectrometry
    Journal of Chromatography A, 1384, 97-106.

  • Ping, L., Xiaoping, D., Yu, Z., Yanli, X., Fei, X., Hailong, Z., Qian, H., Fuqiang, W., Huamin, C., Haihua, W.(2015)
    Polycyclic aromatic hydrocarbons in surface sediment from Yangpu Bay, China: Distribution, sources and risk assessment
    Marine Pollution Bulletin, 1-2, 312-319, doi: 10.1016/j.marpolbul.2015.07.039

  • Rahmanpoor, S., Ghafourian, H., Hashtroudi, S. M., Darvish, B., Kazem, (2014)
    Distribution and sources of polycyclic aromatic hydrocarbons in surface sediments of the Hormuz strait, Persian Gulf
    Marine Pollution Bulletin, 78, pp. 224-229. doi: 10.1016/j.marpolbul.2013.10.032

  • Rascón, A. J., Azzouz, A., & Ballesteros, E. (2019)
    Trace level determination of polycyclic aromatic hydrocarbons in raw and processed meat and fish products from European markets
    by GC-MS.

  • Soltania, N., Moorea, F., Keshavarzia, B., Sorooshianb, A., Javidd, R. (2019)
    Potentially toxic elements (PTEs) and polycyclic aromatic hydrocarbons (PAHs) in fish and prawn in the Persian Gulf, Iran
    Ecotoxicology and Environmental Safety, 173, 251-265.

  • Tavakoly Sany, S. B., Hashim, R., Salleh, A., Rezayi, M., Mehdinia, A., & Safari, O. (2014)
    Polycyclic Aromatic Hydrocarbons in Coastal Sediment of Klang Strait, Malaysia: Distribution Pattern, Risk Assessment and Sources
    PLoS ONE, 9(4), e94907.

  • Wang, Z., Yang, C., Yang, Z., Sun, J., Hollebone, B., Brown, C., & Landriault, M. (2011)
    Forensic fingerprinting and source identification of the 2009 Sarnia (Ontario) oil spill
    Journal of Environmental Monitoring, 13(11), 3004.

  • Keywords

    PAHs, sediments, fish, extraction methods, validation

    Tag search PAHs sediments fish extraction methods validation