Abstract
The procedures of ultrasonic extraction and clean-up were optimized for the determination of polycyclic aromatic hydrocarbons (PAHs) in marine sediments. Samples were ultrasonically extracted, and the extracts were purified with a miniaturized silica gel chromatographic column and analyzed with high performance liquid chromatography (HPLC) with a fluorescence detector. Ultrasonication with methanol-dichloromethane (2:1, v/v) mixture gave higher extraction efficiency than that with dichloromethane. Among the three elution solvents used in clean-up step, dichloromethane-hexane (2:3, v/v) mixture was the most satisfactory. Under the optimized conditions, the recoveries in the range of 54.82% to 94.70% with RSDs of 3.02% to 23.22% for a spiked blank, and in the range of 61.20% to 127.08% with RSDs of 7.61% to 26.93% for a spiked matrix, were obtained for the 15 PAHs studied, while the recoveries for a NIST standard reference SRM 1941b were in the range of 50.79% to 83.78% with RSDs of 5.24% to 21.38%. The detection limits were between 0.75 ng L−1 and 10.99 ng L−1for different PAHs. A sample from the Jiaozhou Bay area was examined to test the established methods.
Similar content being viewed by others
References
Barco-Bonilla, N., Martínez Vidal, J. L., Garrido Frenich, A., and Romero-González, R., 2009. Comparison of ultrasonic and pressurized liquid extraction for the analysis of polycyclic aromatic compounds in soil samples by gas chromatography coupled to tandem mass spectrometry. Talanta, 78(1): 156–164.
Berset, J. D., Ejem, M., Holzer, R., and Lischer, P., 1999. Comparison of different drying, extraction and detection techniques for the determination of priority polycyclic aromatic hydrocarbons in background contaminated soil samples. Analytica Chimica Acta, 383(3): 263–275.
Blankenhorn, I., Meijer, D., and Delft, R. J., 1992. Inter-laboratory comparison of methods used for analysing polycyclic aromatic hydrocarbons (PAHs) in soil samples. Fresenius Journal of Analytical Chemistry, 343(6): 497–504.
Carman, K. R., Fleeger, J. W., Means, J. C., Pomarico, S. M., and McMillin, D. J., 1995. Experimental investigation of the effects of polynuclear aromatic hydrocarbons on an estuarine sediment food web. Marine Environment Research, 40(3): 289–318.
Chee, K. K., Wong, M. K., and Lee, H. K., 1996. Optimization of microwave-assisted solvent extraction of polycyclic aromatic hydrocarbons in marine sediments using a microwave extraction system with high-performance liquid chromatography-fluorescence detection and gas chromatography-mass spectrometry. Journal of Chromatography A, 723(2): 259–271.
Codina, G., Vaquero, M. T., Comellas, L., and Broto-Puig, F., 1994. Comparison of various extraction and clean-up methods for the determination of polycyclic aromatic hydrocarbons in sewage sludge-amended soils. Journal of Chromatography A, 673(1): 21–29.
Filipkowska, A., Lubecki, L., and Kowalewska, G., 2005. Polycyclic aromatic hydrocarbon analysis in different matrices of the marine environment. Analytica Chimica Acta, 547(2): 243–254.
García, A. L., González, E. B., Alonso, J. I. G., and Sanz-Medel, A., 1992. Determination of some Selected Polycyclic Aromatic Hydrocarbons in Environmental Samples by High-Performance Liquid Chromatography with Fluorescence Detection. Chromatographia, 33(5–6): 225–230.
Harkey, G. A., Van Hoof, P. L., and Landrum, P. F., 1995. Bioavailability of PAH from an historically contaminated sediment core. Environmental Toxicology and Chemistry, 14(9): 1551–1560.
Heemken, O. P., Theobald, N., and Wenclawiak, B. W., 1997. Comparison of ASE and SFE with Soxhlet, Sonication, and Methanolic Saponification Extractions for the Determination of Organic Micropollutants in Marine Particulate Matter. Analytical Chemistry, 69(11): 2171–2180.
Janda, V., Bartle, K. D., and Clifford, A. A., 1993. Supercritical fluid extraction in environmental analysis. Journal of Chromatography A, 642(1–2): 283–299.
Kahn, S., Aijun, L., Zhang, S., Hu, Q., and Zhu, Y.G., 2008. Accumulation of polycyclic aromatic hydrocarbons and heavy metals in lettuce grown in the soils contaminated with long-term wastewater irrigation. Journal of Hazardous Materials, 152(2): 506–515.
Lipiatou, E., and Albaigés, J., 1994. Atmospheric deposition of hydrophobic organic chemicals in the northwestern Mediterranean Sea: comparison with the Rhone river input. Marine Chemistry, 46(1–2): 153–164.
Lopez-Avila, V., Young, R., and Beckert, W. F., 1994. Microwave-Assisted Extraction of Organic Compounds from Standard Reference Soils and Sediments. Analytical Chemistry, 66(7): 1097–1106.
Manoli, E., and Samara, C., 1996. Polycyclic Aromatic Hydrocarbons in Waste Waters and Sewage Sludge: Extraction and Clean-up for HPLC Analysis with Fluorescence Detection. Chromatographia, 43(3–4): 135–142.
Miège, C., Dugay, J., and Hennion, M. C., 1998. Optimization and validation of solvent and supercritical-fluid extractions for the trace-determination of polycyclic aromatic hydrocarbons in sewage sludges by liquid chromatography coupled to diode-array and fluorescence detection. Journal of Chromatography A, 823(1–2): 219–230.
Miège, C., Dugay, J., and Hennion, M. C., 2003. Optimization, validation and comparison of various extraction techniques for the trace determination of polycyclic aromatic hydrocarbons in sewage sludges by liquid chromatography coupled to diode-array and fluorescence detection. Journal of Chromatography A, 995(1–2): 87–97.
Navarro, P., Etxebarria, N., and Arana, G., 2009. Development of a focused ultrasonic-assisted extraction of polycyclic aromatic hydrocarbons in marine sediment and mussel samples. Analytica Chimica Acta, 648(2): 178–182.
Neff, J. M., 1979. Polycyclic Aromatic Hydrocarbons in the Aquatic Environment: Sources, Fates, and Biological Effects. Applied Science Publishers, London, 89–92.
Popp, P., Keil, P., Moder, M., Paschke, A., and Thuss U., 1997. Application of accelerated solvent extraction followed by gas chromatography, high-performance liquid chromatography and gas chromatography-mass spectrometry for the determination of polycyclic aromatic hydrocarbons, chlorinated pesticides and polychlorinated dibenzo-p-dioxins and dibenzofurans in solid wastes. Journal of Chromatography A, 774(9): 203–211.
Richter, B. E., Jones, B. A., Ezzell, J. L., Porter, N. L., Avdalovic, N., and Pohl, C., 1996. Accelerated solvent extraction: a technique for sample preparation. Analytical Chemistry, 68(6): 1033–1039.
Stegeman, J. J., and Lech, J. J., 1991. Cytochrome P-450 mono-oxygenase systems in aquatic species: Carcinogen metabolism and biomarkers for carcinogen and pollutant exposure. Environmental Health Perspectives, 90: 101–109.
Sun, F., Littlejohn, D., and Gibson, M. D., 1998. Ultrasonication extraction and solid phase extraction clean-up for determination of US EPA 16 priority pollutant polycyclic aromatic hydrocarbons in soils by reversed-phase liquid chromatography with ultraviolet absorption detection. Analytica Chimica Acta, 364(1–3): 1–11.
Vannoort, R. W., Chervet, J. P., Lingeman, H., De Jong, G. J., and Brinkman., U. A. T., 1990. Coupling of supercritical fluid extraction with chromatographic techniques. Journal of Chromatography, 505(1): 45–77.
Wenclawiak, B., Rathmann, C., and Teuber, A., 1992. Supercritical fluid extraction of soil samples and determination of polycyclic aromatic hydrocarbons (PAHs) by HPLC. Fresenius Journal of Analytical Chemistry, 344(10–11): 497–500.
Witt, G., 1995. Polycyclic aromatic hydrocarbons in water and sediment of the Baltic sea. Marine Pollutution Bulletin, 31(4): 237–248.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Peng, X., Yan, G., Li, X. et al. Optimization of ultrasonic extraction and clean-up protocol for the determination of polycyclic aromatic hydrocarbons in marine sediments by high-performance liquid chromatography coupled with fluorescence detection. J. Ocean Univ. China 11, 331–338 (2012). https://doi.org/10.1007/s11802-012-1846-5
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s11802-012-1846-5