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 |
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| Authors: | Xuewei Peng Guofang Yan Xianguo Li Xinyun Guo Xiao Zhou Yan Wang |
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| Institution: | 1) 1) Key Laboratory of Marine Chemistry Theory and Technology, Ministry of Education, Ocean University of China, Qingdao 266100, P. R. China 2) College of Chemistry and Chemical Engineering, Weifang College, Weifang 261061, P. R. China 3) Qingdao Supervision and Testing Center of Product Quality, Qingdao 266061, P. R. China 4) General Administration of Quality Supervision, Inspection and Quarantine of the People’s Republic of China, Beijing 100088, P. R. China |
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| 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. |
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