Department of Chemistry, East China Normal University, Shanghai, 200241, P. R. China.
Analyst. 2011 Oct 7;136(19):3988-96. doi: 10.1039/c1an15245a. Epub 2011 Aug 17.
Solid-phase extraction (SPE) is one of the most important techniques for sample preparation, purification, concentration and cleanup. Membranes made from synthetic organic polymers, cellulose, or glass fibers are used for sample pretreatment. In this work, we report that a porous metal membrane, the metal filter in HPLC, was used as a novel kind of solid-phase extraction adsorbent material. To evaluate the performance of the porous metal membrane for the SPE, naphthalene, fluorene, anthracene, phenanthrene, fluoranthene, pyrene, chrysene, perylene and benzo(a)pyrene were selected as analytes. Several parameters that affected the extraction efficiency such as the extraction time, the concentration of NaCl, the extraction temperature and the agitation speed were optimized. The experimental result indicates that the porous metal membrane possesses high adsorption ability to the tested polycyclic aromatic hydrocarbons (PAHs). Under the optimum conditions, the detection limits of the developed method were in the range of 0.03-0.082 μg L(-1) (S/N = 5), and excellent linear correlations between peak area and concentration of PAHs were found over the range of 0.1-60 μg L(-1). The precisions (RSD) for five replicate extractions of the PAHs from sample solutions were in the range of 2.6-5.0%. The recoveries of the PAHs from tap water and river water samples spiked with 9 PAHs (20 μg L(-1) of each individual PAH) ranged from 83.0% to 112.5%. The porous metal membrane is durable, simple, inexpensive, reproducible and has a high adsorption ability for use in SPE of PAHs.
固相萃取（SPE）是样品制备、净化、浓缩和清洗的最重要技术之一。用于样品预处理的膜由合成有机聚合物、纤维素或玻璃纤维制成。在这项工作中，我们报告了一种多孔金属膜，即 HPLC 中的金属过滤器，可用作新型固相萃取吸附材料。为了评估多孔金属膜对 SPE 的性能，选择萘、芴、蒽、菲、荧蒽、芘、屈、苝和苯并（a）芘作为分析物。优化了影响萃取效率的几个参数，如萃取时间、NaCl 浓度、萃取温度和搅拌速度。实验结果表明，多孔金属膜对测试的多环芳烃（PAHs）具有高吸附能力。在最佳条件下，所开发方法的检测限在 0.03-0.082 μg L(-1)（S/N = 5）范围内，并且在 0.1-60 μg L(-1) 范围内发现了峰面积与 PAHs 浓度之间的优异线性相关性。从样品溶液中五次重复萃取 PAHs 的精密度（RSD）在 2.6-5.0%范围内。从自来水和河水样品中加入 9 种 PAHs（每种 PAH 的浓度为 20 μg L(-1)）萃取的 PAHs 的回收率范围为 83.0%-112.5%。多孔金属膜耐用、简单、价格低廉、可重复使用，对 PAHs 的 SPE 具有高吸附能力。
