Department of Marine Chemistry, Faculty of Marine Science, Khorramshahr University of Marine Science and Technology, Khorramshahr, Iran.
Anal Chim Acta. 2012 Feb 10;714:89-97. doi: 10.1016/j.aca.2011.11.065. Epub 2011 Dec 8.
The application of sulfur microparticles as efficient adsorbents for the solid-phase extraction (SPE) and determination of trace amounts of 10 polycyclic aromatic hydrocarbons (PAHs) was investigated in sea water and wastewater samples using high performance liquid chromatography coupled with an ultraviolet detector (HPLC-UV). Parameters influencing the preconcentration of PAHs such as the amount of sulfur, solution flow rate and volume, elution solvent, type and concentration of organic modifier, and salt effect were examined. The results showed that at a flow rate of 10 mL min(-1) for the sample solutions (100mL), the PAHs could be adsorbed on the sulfur microparticles and then eluted by 2.0 mL of acetonitrile. For HPLC-UV analysis of extracted PAHs, the calibration curves were linear in the range of 0.05-80.0 μg L(-1); the coefficients of determinations (r(2)) were between 0.9934 and 0.9995. The relative standard deviations (RSDs) for eight replicates at two concentration levels (0.5 and 4.0 μg L(-1)) of PAHs were lower than 7.3%, under optimized conditions. The limits of detection (LODs, S/N = 3) of the proposed method for the studied PAHs were 0.007-0.048 μg L(-1). The recoveries of spiked PAHs (0.5 and 4 μg L(-1)) in the wastewater and sea water samples ranged from 78% to 108%. The simplicity of experimental procedure, high extraction efficiency, short sample analysis, and using of low cost sorbent demonstrate the potential of this approach for routine trace PAH analysis in water and wastewater samples.
研究了将硫微球作为高效吸附剂应用于固相萃取（SPE）和高效液相色谱-紫外检测法（HPLC-UV）测定海水中痕量 10 种多环芳烃（PAHs）的方法。考察了影响 PAHs 预浓缩的参数，如硫的用量、溶液流速和体积、洗脱溶剂、有机改性剂的类型和浓度以及盐效应。结果表明，在样品溶液（100 mL）流速为 10 mL min(-1)时，PAHs 可被硫微球吸附，然后用 2.0 mL 乙腈洗脱。对于提取的 PAHs 的 HPLC-UV 分析，校准曲线在 0.05-80.0 μg L(-1)范围内呈线性；相关系数（r(2)）在 0.9934 到 0.9995 之间。在优化条件下，两种浓度（0.5 和 4.0 μg L(-1))的 PAHs 重复 8 次的相对标准偏差（RSD）低于 7.3%。该方法对研究中的 PAHs 的检出限（LOD，S/N = 3）为 0.007-0.048 μg L(-1)。在废水和海水中，加标 PAHs（0.5 和 4 μg L(-1))的回收率在 78%-108%之间。该方法实验步骤简单、萃取效率高、样品分析时间短、使用成本低，展示了其在水和废水样品中常规痕量 PAH 分析的潜力。
