State Key Laboratory of Chemo/Biosensing & Chemometrics, College of Chemistry & Chemical Engineering, Hunan University, Changsha 410082, China.
Analyst. 2013 Oct 21;138(20):5904-12. doi: 10.1039/c3an01027a. Epub 2013 Aug 9.
A novel sorbent for magnetic solid-phase extraction, 1,4,7,10-tetrabenzyl-1,4,7,10-tetraazacyclododecane (TBCD) modified magnetic nanoparticles, was synthesized in this work. The four benzyl groups of TBCD provide the Fe3O4-TBCD nanoparticles with strong adsorption capacity for polycyclic aromatic hydrocarbons (PAHs) due to their π-π stacking interaction, which increases selectivity of the synthesized material to target analytes. The prepared material was characterized by scanning electron microscopy, X-ray diffraction patterns, Fourier transform infrared spectroscopy and vibrating sample magnetometry. The results indicated that the Fe3O4-TBCD nanoparticles were successfully prepared, and the particles were homogeneous nanospheres with excellent magnetic properties. Based on the optimized extraction conditions, a rapid and effective method was developed for the pre-concentration of PAHs from environmental water samples by combination with high performance liquid chromatography (HPLC). Satisfactory precision and accuracy of the developed method were obtained in a low concentration range of 0.3 ng L(-1) to 1.2 × 10(3) ng L(-1). This method produced lower limits of detection in the range of 3.0 × 10(-2) ng L(-1) to 1.2 ng L(-1). The high pre-concentration rate and efficiency of the method ensure its successful application in extraction of trace PAHs from large volumes of environmental water samples. The extraction recoveries in environmental water samples ranged from 81.1% to 115.5% with the relative standard deviations (n = 5) less than 10%.
一种新型的用于磁性固相萃取的吸附剂，1,4,7,10-四苄基-1,4,7,10-四氮杂环十二烷（TBCD）修饰的磁性纳米粒子，在本工作中被合成。TBCD 的四个苄基基团由于其π-π堆积相互作用，为 Fe3O4-TBCD 纳米粒子提供了对多环芳烃（PAHs）的强吸附能力，这增加了合成材料对目标分析物的选择性。通过扫描电子显微镜、X 射线衍射图谱、傅里叶变换红外光谱和振动样品磁强计对制备的材料进行了表征。结果表明，成功制备了 Fe3O4-TBCD 纳米粒子，且粒子为具有优异磁性的均匀纳米球。基于优化的萃取条件，通过与高效液相色谱（HPLC）联用，建立了一种从环境水样中预浓缩 PAHs 的快速有效的方法。在所研究的低浓度范围内（0.3 ng L(-1) 至 1.2 × 10(3) ng L(-1)），该方法获得了令人满意的精密度和准确度。该方法的检出限范围为 3.0 × 10(-2) ng L(-1) 至 1.2 ng L(-1)。该方法的高浓缩率和高效率确保了其在从大量环境水样中提取痕量 PAHs 方面的成功应用。在环境水样中的萃取回收率在 81.1%至 115.5%之间，相对标准偏差（n = 5）小于 10%。
