Department of Applied Chemistry, National University of Kaohsiung, No. 700, Kaohsiung University Road, Nan Tzu District, Kaohsiung 811, Taiwan.
J Chromatogr A. 2010 Mar 5;1217(10):1647-53. doi: 10.1016/j.chroma.2010.01.032. Epub 2010 Jan 18.
This paper describes the use of reversed-phase liquid chromatography (RPLC) to rapidly characterize Au/Pt core/shell nanoparticles (NPs) produced through seed-assisted synthesis. We monitored the sizes of Au/Pt core/shell NPs by using a porous silica-based RPLC column (pore size: ca. 100 nm) and 30 mM sodium dodecyl sulfate in deionized water as the mobile phase; the plot of the retention time with respect to the logarithm of the size of the Au NPs was linear (R(2)=0.997) for diameters falling in the range from 5.3 to 40.1 nm; from five consecutive runs, the relative standard deviations of these retention times were less than 0.4%. We used the optimal separation conditions of the RPLC system to study the effects that the rate of addition of the reducing agent and the volumes of the seed, shell precursor metal ion, and reducing agent solutions had on the sizes of the Au/Pt core/shell NPs. A good correlation existed between the sizes of the Au/Pt core/shell NPs determined through RPLC and those determined using transmission electron microscopy. RPLC appears to be a useful technique for monitoring the sizes of NPs and nanomaterials in general.
本文描述了反相液相色谱(RPLC)在通过种子辅助合成快速表征 Au/Pt 核壳纳米粒子(NPs)中的应用。我们使用基于多孔硅的 RPLC 柱(孔径:约 100nm)和 30mM 十二烷基硫酸钠在去离子水中作为流动相来监测 Au/Pt 核壳 NPs 的尺寸;Au NPs 尺寸的保留时间与尺寸的对数之间的关系呈线性(R²=0.997),直径范围为 5.3nm 至 40.1nm;从连续五次运行中,这些保留时间的相对标准偏差小于 0.4%。我们使用 RPLC 系统的最佳分离条件来研究还原剂的添加速率以及种子、壳前体金属离子和还原剂溶液的体积对 Au/Pt 核壳 NPs 尺寸的影响。通过 RPLC 确定的 Au/Pt 核壳 NPs 的尺寸与通过透射电子显微镜确定的尺寸之间存在良好的相关性。RPLC 似乎是一种用于监测 NPs 和纳米材料一般尺寸的有用技术。