Qu Qi-Shu, Zhang Xin-Xin, Zhao Zhen-Zhen, Hu Xiao-Ya, Yan Chao
College of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou 225002, China.
J Chromatogr A. 2008 Jul 11;1198-1199:95-100. doi: 10.1016/j.chroma.2008.05.036. Epub 2008 May 22.
Monodispersed spherical gold particles synthesized and modified with n-octadecanethiol (C18-Au) were packed into a 100 microm I.D. capillary column and tested in capillary high-performance liquid chromatography (microHPLC). To the best of our knowledge, this represents the first report on the actual use of micron gold particles as stationary phase in a packed column microHPLC. As measured by scanning electron microscopy, the average diameter of these gold microspheres was 3.5 microm and the surface area, average pore diameter, and average pore volume were 49.4m(2)/g, 4.8 nm, and 0.12 cm(3)/g, respectively. The retention behavior of neutral compounds on the n-octadecanethiol-modified gold microspheres was investigated by separating a mixture of small organic compounds using microHPLC. The results from the experiments show that C18-Au behaves basically as a reversed phase. The test of chemical stability of the C18-Au stationary phase under alkaline condition demonstrates that it is stable with the flushing of a mobile phase at pH 12 for at least 140 h. The C18-Au particles are also mechanically strong enough to withstand pressure up to 52 MPa. The preliminary results in this work prove the feasibility of the fabrication of C18-Au micron particles as a novel stationary phase for packed column microHPLC.
用正十八烷硫醇（C18 - Au）合成并修饰的单分散球形金颗粒被填充到内径为100微米的毛细管柱中，并在毛细管高效液相色谱（微型HPLC）中进行测试。据我们所知，这是关于在填充柱微型HPLC中实际使用微米级金颗粒作为固定相的首次报道。通过扫描电子显微镜测量，这些金微球的平均直径为3.5微米，表面积、平均孔径和平均孔体积分别为49.4平方米/克、4.8纳米和0.12立方厘米/克。通过微型HPLC分离小有机化合物混合物，研究了中性化合物在正十八烷硫醇修饰的金微球上的保留行为。实验结果表明，C18 - Au基本表现为反相。C18 - Au固定相在碱性条件下的化学稳定性测试表明，在pH 12的流动相冲洗至少140小时的情况下它是稳定的。C18 - Au颗粒的机械强度也足以承受高达52兆帕的压力。这项工作的初步结果证明了制备C18 - Au微米颗粒作为填充柱微型HPLC新型固定相的可行性。
