Schuetze Benjamin, Mayer Christian, Loza Kateryna, Gocyla Martin, Heggen M, Epple Matthias
Inorganic Chemistry and Center for Nanointegration Duisburg-Essen (CeNIDE), Universitaetsstr. 5-7, 45117 Essen, Germany.
J Mater Chem B. 2016 Mar 28;4(12):2179-2189. doi: 10.1039/c5tb02443a. Epub 2016 Mar 4.
Gold nanoparticles, functionalized by aliphatic and aromatic mercapto-functionalized carboxylic acids and by two small peptides (CG and CGGRGD), respectively, were synthesized by the reduction of HAuCl with NaBH in the presence of the above ligands. After purification by centrifugation or filtration and redispersion, the dispersed nanoparticles were analysed by differential centrifugal sedimentation (DCS), high-resolution transmission electron microscopy (HRTEM), and a variety of NMR spectroscopic techniques: H-NMR, H,H-COSY and H-DOSY. The hydrodynamic diameter of the particles was between 1.8 and 4.4 nm, as determined by DOSY, in good agreement with the DCS and HRTEM results. Diffusion ordered spectroscopy (DOSY) turned out to be a valuable and non-destructive tool to determine the hydrodynamic diameter of dispersed nanoparticles and to control the purity of the final particles. The coordination of the organic molecules to the gold nanoparticles resulted in distinct and complex changes in the H-NMR spectra. These were only partially explainable but clearly caused by the vicinity of the molecules to the gold nanoparticle.
分别用脂肪族和芳香族巯基官能化的羧酸以及两种小肽（CG和CGGRGD）对金纳米颗粒进行功能化处理，在上述配体存在的情况下，通过用硼氢化钠还原氯金酸来合成。经过离心或过滤纯化以及再分散后，通过差示离心沉降（DCS）、高分辨率透射电子显微镜（HRTEM）以及多种核磁共振光谱技术：氢核磁共振（¹H-NMR）、¹H,¹H-COSY和¹H-DOSY对分散的纳米颗粒进行分析。通过扩散排序光谱法（DOSY）测定，颗粒的流体动力学直径在1.8至4.4纳米之间，这与DCS和HRTEM的结果高度吻合。扩散排序光谱法（DOSY）被证明是一种有价值的非破坏性工具，可用于确定分散纳米颗粒的流体动力学直径并控制最终颗粒的纯度。有机分子与金纳米颗粒的配位导致¹H-NMR光谱发生明显而复杂的变化。这些变化只能部分得到解释，但显然是由分子与金纳米颗粒的接近程度引起的。
