AJAC  Vol.2 No.7 , November 2011
Multifactorial Optimization Approach for Determination of Polycyclic Aromatic Hydrocarbons in Sea Sediments of Turkish Mediterranean Coast
Abstract: Present study aims the optimisation and validation of the extraction procedures for the determination of poly- cyclic aromatic hydrocarbons (PAHs) in sediment samples. As analytical techniques, gas chromatography- mass detector (GC-MS) and gas chromatography-flame ionization detector (GC-FID). The optimized methods were soxhlet extraction, ultrasonic bath extraction and solid phase micro extraction (SPME). The factorial design was used in order to search out the main factors affecting extraction efficiencies. The best extraction method was chosen as ultrasonic bath extraction and optimum values for main factors were selected for the development of this extraction method. The optimised methods were validated to confirm the reliability. Percent errors were in between 1.40% - 25.0%. Relative standard deviation was less than 1% and limit of detection changed from 0.006 to 0.028 mg/L. The accuracy of the method was verified by analyzing National Institute of Standards and Technology, Standard Reference Material 1597a (NIST SRM 1597a). The selectivity, accuracy and precision were quite adequate for the determination of PAHs in sediment samples. The best extraction and analysis methods were then applied to determine 16 PAHs in sea sediments from Ölüdeniz Lagoon, of Turkish Meditreanean coast and marine sediment, SRM 1941b. The highest observed cocentration for PAHs was 0.620 mg?kg–1 for Acenaphtene.Total sum of the concentrations for all the observed PAHs was1.854 mg?kg–1.
Cite this paper: nullS. Tuncel and T. Topal, "Multifactorial Optimization Approach for Determination of Polycyclic Aromatic Hydrocarbons in Sea Sediments of Turkish Mediterranean Coast," American Journal of Analytical Chemistry, Vol. 2 No. 7, 2011, pp. 783-794. doi: 10.4236/ajac.2011.27090.

[1]   J. Xu, Y. Yu, P. Wang, W. Guo, S. Dai and H. Sun, “Polycyclic Aromatic Hydrocarbons in the Surface Sedi- ments from Yellow River, China,” Chemosphere, Vol. 67, No. 7, 2007, pp. 1408-1414. doi:10.1016/j.chemosphere.2006.10.074

[2]   L. Culotta, C. D. Stefano, A. Gianguzza, M. R. Mannino and S. Orecchio, “The PAH Composition of Surface Sedi- ments from Stagnone Coastal Lagoon, Marsala (Italy),” Marine Chemistry, Vol. 99, No. 1-4, 2006, pp. 117-127. doi:10.1016/j.marchem.2005.05.010

[3]   Y. F. Song, X. Jing, S. Fleischmann and B. M. Wilke, “Comparative Study of Extraction Methods for the Deter- mination of PAHs from Contaminated Soils and Sedi- ments,” Chemosphere, Vol. 48, No. 9, 2002, pp. 993- 1001. doi:10.1016/S0045-6535(02)00180-7

[4]   N. F. Leite, P. P. Zamora and M. T. Grassi, “Multifactorial Optimization Approach for the Determi- nation of Polycyclic Aromatic Hydrocarbons in River Sediments by Gas Chromatography-Quadrupole ?on Trap Selected ?on Storage Mass Spectrometry,” Journal of Chromatography A, Vol. 1192, No. 2, 2008, pp. 273-281. doi:10.1016/j.chroma.2008.03.067

[5]   M. B Deschamps, J. J. Daudin and E. Barriuso, “An Experimental Design Approach to Optimise the Determi- nation of Polycyclic Aromatic Hydrocarbons from Rainfall Water Using Stir Bar Sorptive Extraction and High Performance Liquid Chromatography-Fluorescence Detection,” Journal of Chromatography A, Vol. 1167, No. 2, 2007, pp. 143-153. doi:10.1016/j.chroma.2007.08.025

[6]   C. R. T. E. Tarley, G. Silveira, W. N. L. Santos, G. D. Matos, E. G. P. Silva, M. A. Bezerra, M. Miró and S. L. C. Ferreira, “Chemometric Tools in Electro Analytical Chemistry: Methods for Optimization Based on Factorial Design and Response Surface Methodology,” Micro chemical Journal, Vol. 92, No. 1, 2009, pp. 58-67. doi:10.1016/j.microc.2009.02.002

[7]   J. N. Miller and J. C. Miller, “Statistics and Chemometrics for Analytical Chemistry,” 4th Edition, Pearson Education, England, 2000, Chapter 7.

[8]   B. E. Berg, H. S. Lund, A. Kringstad and A. L. Kvern- heim, “Routine Analysis of Hydrocarbons, PCB and PAH in Marine Sediments Using Supercritical CO2 Extraction,” Chemosphere, Vol. 38, No. 3, 1999, pp. 587-599. doi:10.1016/S0045-6535(98)00213-6

[9]   D. R. Banjoo and P. K. Nelson, “Improved Ultrasonic Extraction Procedure for the Determination of Polycyclic Aromatic Hydrocarbons in Sediments,” Journal of Chro- matography A, Vol. 1066, No. 1-2, 2005, pp. 9-18. doi:10.1016/j.chroma.2005.01.033

[10]   H. Budzinski, M. Letellier, P. Garrigues and K. Le Men- ach, “Optimisation of the Microwave-Assisted Extraction in Open Cell of Polycyclic Aromatic Hydrocarbons from Soils and Sediments: Study of Moisture Effect,” Journal of Chromatography A, Vol. 837, No. 1-2, 1999, pp. 187- 200. doi:10.1016/S0021-9673(99)00067-9

[11]   EPA METHOD 3540 C, 1996.

[12]   EPA METHOD SW-846 3550C, 2007.

[13]   EPA METHOD 3550 B, 1996.

[14]   A. Nikolaou, M. Kostopoulou, G. Lofrano and S. Meric, “Determination of PAHs in Marine Sediments: Analytical Methods and Environmental Concerns,” Global Nest Journal, Vol. 11, 2009, pp. 391-405.

[15]   C. Anyakora, A. Ogbeche, P. Palmer, H. Coker, G. Ukpo and C. Ogah, “GC/MS Analysis of Polynuclear Aromatic Hydrocarbons in Sediment Samples from the Niger Delta Region,” Chemosphere, Vol. 60, No. 7, 2005, pp. 990- 997. doi:10.1016/j.chemosphere.2004.12.073

[16]   R. Boonyatumanond, G. Wattayakorn, A. Togo and H. Takada, “Distribution and Origins of Polycyclic Aromatic Hydrocarbons (PAHs) in Riverine, Estuarine and Marine Sediments in Thailand”, Marine Pollution Bulletin, Vol. 52, No. 8, 2006, pp. 942-956. doi:10.1016/j.marpolbul.2005.12.015

[17]   C. H. Koch, J. S. Khim, D. L. Villeneuve , K. Kannan and J. P. Giesy, “Characterization of Trace Organic Con-taminants in Marine Sediment from Yeongil Bay, Korea: 1. Instrumental Analyses,” Environmental Pollution, Vol. 142, No. 1, 2006, pp. 39-47. doi:10.1016/j.envpol.2005.09.005

[18]   A. Filipkowska, L. Lubecki and G. Kowalewska, “Poly- cyclic Aromatic Hydrocarbon Analysis in Different Matri- ces of the Marine Environment,” Analytica Chimica Acta, Vol. 547, No. 2, 2005, pp. 243-254. doi:10.1016/j.aca.2005.05.023

[19]   V. Librando, O. Hutzinger, G. Tringali and M. Aresta, “Supercritical Fluid Extraction of Polycyclic Aromatic Hy- drocarbons from Marine Sediments and Soil Samples,” Chemosphere, Vol. 54, No. 8, 2004, pp. 1189-1197. doi:10.1016/j.chemosphere.2003.07.008

[20]   R. A. Gimeno, E. Comas, R. M. Marcé, J. Ferré, F. X. Rius and F. Borrull, “Second-Order Bilinear Calibration for De- termining Polycyclic Aromatic Compounds in Marine Sediments by Solvent Extraction and Liquid Chromatography with Diode-Array Detection,” Analytica Chimica Acta, Vol. 498, No. 1-2, 2003, pp. 47-53. doi:10.1016/j.aca.2003.08.057

[21]   V. Pino, J. H. Ayala, A. M. Afonso and V. Gonzalez, “Micellar Microwave-Assisted Extraction Combined with Solid-Phase Microextraction for the Determination of Polycyclic Aromatic Hydrocarbons in a Certified Marine Sediment,” Analytica Chimica Acta, Vol. 477, No. 1, 2003, pp. 81-91. doi:10.1016/S0003-2670(02)01410-1