TY - JOUR ID - 375 TI - Improved Analytical Extraction and Clean-up Techniques for the Determination of PAHs in Contaminated Soil Samples JO - International Journal of Environmental Research JA - IJER LA - en SN - 1735-6865 AU - Oluseyi, T. AU - Olayinka, K. AU - Alo, B. AU - Smith, R.M. AD - Department of Chemistry, University of Lagos, Akoka, Yaba, Nigeria AD - Department of Chemistry, Loughborough University, Leicestershire, UK Y1 - 2011 PY - 2011 VL - 5 IS - 3 SP - 681 EP - 690 KW - PAHs KW - Soil KW - Solid phase extraction KW - HPLC KW - Ultra sonication DO - 10.22059/ijer.2011.375 N2 - Development and optimisation of fast, efficient, quantitative, economic and environmentally friendly analytical extraction techniques for the extraction clean up, and pre-concentration in the quantification of 16 USEPA priority polycyclic aromatic hydrocarbons (PAHs) in contaminated soils have been carried out. Three different extraction methods (Soxhlet, ultra sonication and mechanical shaking) were investigated on a low-level PAH soil certified reference material (CRM131-100) and the results were compared to determine the technique with the highest extraction efficiency. The clean up and pre-concentration procedures were optimized using both the conventional method (i.e. column packing with silica gel) as well as the solid phase extraction (SPE). Chromatographic conditions for the separation of PAHs using High Performance Liquid Chromatography (HPLC) using UV-DAD and fluorimetric detection with programmed excitation and emission wavelengths were also optimized. Six different extraction solvents: acetone, cyclohexane, 2- propanol, methanol, acetonitrile and dichloromethane, were tested to select the most suitable solvent for the extraction of the 16 PAHs from the certified soil reference material. Acetonitrile, dichloromethane and tetrahydrofuran were also tested as eluants for the optimisation of SPE clean up. The optimized ultrasonic extraction procedure utilizing four 15 minutes extraction cycles at 50 ÂșC and SPE clean up with tetrahydrofuran: acetonitrile (1:1) and subsequent separation by gradient reversed phase HPLC with fluorimetric detection extracted the PAHs from the certified reference material with recoveries ranging from 63.6 % to over 100 % . UR - https://ijer.ut.ac.ir/article_375.html L1 - https://ijer.ut.ac.ir/article_375_2cbec312063748e3bfb8e59dc5223350.pdf ER -