Department of Chemistry, College of Science, Agricultural University of Hebei, Baoding 071001, China.
J Chromatogr A. 2013 Jun 7;1293:20-7. doi: 10.1016/j.chroma.2013.03.071. Epub 2013 Apr 9.
In this paper, a magnetic microsphere-confined graphene adsorbent (Fe3O4@SiO2-G) was fabricated and used for the extraction of five polycyclic aromatic hydrocarbons (fluorene, anthracene, phenanthrene, fluoranthene and pyrene) from environmental water samples prior to high performance liquid chromatography with fluorescence detection. The Fe3O4@SiO2-G was characterized by various instrumental methods. Various experimental parameters that could affect the extraction efficiencies, such as the amount of Fe3O4@SiO2-G, the pH and ionic strength of sample solution, the extraction time and the desorption conditions, were investigated. Due to the high surface area and excellent adsorption capacity of the Fe3O4@SiO2-G, satisfactory extraction can be achieved with only 15mg of the adsorbent per 250mL solution and 5min extraction. Under the optimum conditions, a linear response was observed in the concentration range of 5-1500ngL(-1) for fluorene, 2.5-1500ngL(-1) for anthracene and 15-1500ngL(-1) for phenanthrene, fluoranthene and pyrene, with the correlation coefficients (r) ranging from 0.9897 to 0.9961. The limits of detection (S/N=3) of the method were between 0.5 and 5.0ngL(-1). The relative standard deviations (RSDs) were less than 5.6%. The recoveries of the method were in the range between 83.2% and 108.2%. The results indicated that this graphene-based magnetic nanocomposite had a great adsorptive ability toward the five polycyclic aromatic hydrocarbons from environmental water samples.
本文制备了一种磁性微球限域的石墨烯吸附剂(Fe3O4@SiO2-G),并将其用于环境水样中 5 种多环芳烃(芴、蒽、菲、荧蒽和芘)的萃取,萃取后采用高效液相色谱-荧光检测法进行分析。采用多种仪器方法对 Fe3O4@SiO2-G 进行了表征。考察了各种实验参数,如 Fe3O4@SiO2-G 的用量、样品溶液的 pH 值和离子强度、萃取时间和解吸条件等,这些参数会影响萃取效率。由于 Fe3O4@SiO2-G 具有高比表面积和优异的吸附能力,仅需 15mg 吸附剂即可对 250mL 溶液进行萃取,萃取时间为 5min 即可达到满意的萃取效果。在最佳条件下,芴、蒽和菲、荧蒽和芘的浓度在 5-1500ngL(-1)、2.5-1500ngL(-1)和 15-1500ngL(-1)范围内均呈现良好的线性响应,相关系数(r)范围为 0.9897-0.9961。该方法的检出限(S/N=3)在 0.5-5.0ngL(-1)之间。相对标准偏差(RSD)小于 5.6%。方法的回收率在 83.2%-108.2%之间。结果表明,这种基于石墨烯的磁性纳米复合材料对环境水样中的 5 种多环芳烃具有很强的吸附能力。