School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou, China.
Anal Chem. 2013 Jul 16;85(14):6885-93. doi: 10.1021/ac4011364. Epub 2013 Jun 28.
A facile and efficient strategy about the synthesis of a novel kind of hybrid magnetic metal-organic framework (MOF)-5 via chemical bonding assembly was reported. The covalent bonding established between the amino functionalized Fe3O4 nanoparticles and the surface of the metal organic framework improved the chemical stability and structure uniformity of the hybrid microcrystals. Combination of MOF-5 with Fe3O4 nanoparticles allows for facile withdrawal of the porous materials by magnetic decantation. The powder X-ray diffraction patterns of the hybrid magnetic MOF-5 showed the structure of the metal organic framework was not disturbed with the decoration of magnetic nanoparticles. The as-synthesized materials combine the favorable attributes of both magnetic characteristics of Fe3O4 nanoparticles and high porosity of metal organic framework, making them excellent candidates as adsorbents for magnetic enrichment of trace analytes. Their potential applications were explored by preconcentrating polycyclic aromatic hydrocarbons and gibberellic acids from environmental, food, and plant samples prior to gas chromatography-mass spectrometry (GC/MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS), respectively. The results showed that the magnetic MOF-5 exhibited superior enrichment capacity for both of these nonpolar and polar analytes. The method demonstrated good precision (relative standard deviations (RSDs) of 1.7-9.7%), low detection limits (0.91-1.96 ng·L(-1) for polycyclic aromatic hydrocarbons and 0.006-0.08 μg L(-1) for gibberellic acid), and good linearity (correlation coefficients higher than 0.9949). The RSDs of batch-to-batch extraction were 2.9-11.2%. The magnetic MOF-5 was robust enough for repeatable use without damage of extraction performance.
一种通过化学键合组装合成新型杂化磁性金属有机骨架（MOF）-5 的简便高效策略被报道。氨基功能化 Fe3O4 纳米粒子与金属有机骨架表面之间建立的共价键提高了杂化微晶体的化学稳定性和结构均一性。MOF-5 与 Fe3O4 纳米粒子的结合使得多孔材料可以通过磁倾析轻松去除。杂化磁性 MOF-5 的粉末 X 射线衍射图谱表明，金属有机骨架的结构在磁性纳米粒子的修饰下没有受到干扰。所合成的材料结合了 Fe3O4 纳米粒子的磁性和金属有机骨架的高孔隙率的优点，使它们成为痕量分析物磁性富集的优秀吸附剂。通过分别对环境、食品和植物样品中的多环芳烃和赤霉素进行预浓缩，然后进行气相色谱-质谱（GC/MS）和液相色谱-串联质谱（LC-MS/MS），探索了它们的潜在应用。结果表明，磁性 MOF-5 对这两种非极性和极性分析物都表现出优异的富集能力。该方法表现出良好的精密度（多环芳烃的相对标准偏差（RSD）为 1.7-9.7%，赤霉素的检测限为 0.91-1.96ng·L-1 和 0.006-0.08μg·L-1）和良好的线性（相关系数均高于 0.9949）。批间萃取的 RSD 为 2.9-11.2%。磁性 MOF-5 足够坚固，可以重复使用而不会损坏萃取性能。
