Optimization of Ultrasonic Extraction and Clean-up Protocol for the Determination of Polycyclic Aromatic Hydrocarbons in Marine Sediments by High-performance Liquid Chroma-tography Coupled with Fluorescence Detection  

作　　者：PENG Xuewei YAN Guofang LI Xianguo GUO Xinyun ZHOU Xiao WANG Yan 

机构地区：[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

出　　处：《Journal of Ocean University of China》2012年第3期331-338,共8页中国海洋大学学报（英文版）

基　　金：supported by the National Natural Science Foundation of China (Grant No.20775074)

摘　　要：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.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.

关 键 词：ultrasonic extraction marine sediment polycyclic aromatic hydrocarbon high performance liquid chromatography 

分 类 号：O657.72[理学—分析化学] TS255.4[理学—化学]