Zhou Li, Jiang Shenmeng, Zhang Xue, Fang Linlin, Guo Xingjie
Shenyang Pharmaceutical University, Shenyang, Liaoning Province, P. R. China.
Electrophoresis. 2018 Apr;39(7):941-947. doi: 10.1002/elps.201700462. Epub 2018 Jan 30.
In this paper, β-cyclodextrin (β-CD) modified gold nanoparticles (AuNPs) coated open tubular column (OT column) was prepared for capillary electrochromatography. The open tubular column was constructed through self-assembly of gold nanoparticles on 3-mercaptopropyl-trimethoxysilane (MPTMS) prederivatized capillary and subsequent modification of thiols β-cyclodextrin (SH-β-CD). Scanning electron microscopy (SEM), transmission electron microscopy (TEM) and ultraviolet visible spectroscopy were carried out to characterize the prepared open tubular column and synthesized gold nanoparticles. By comparing different coating times of gold nanoparticles and thiols β-cyclodextrin, we got the optimal conditions for preparing the open tubular column. Also, the separation parameters were optimized including buffer pH, buffer concentration and applied voltage. Separation effectiveness of open tubular column was verified by the separation of four pairs of drug enantiomers including bifonazole, fexofenadine, omeprazole and lansoprazole, and satisfactory separation results were achieved for these analytes studied. In addition, the column showed good stability and repeatability. The relative standard deviation values less than 5% were obtained through intra-day, inter-day, and column-to-column investigations.
本文制备了用于毛细管电色谱的β-环糊精（β-CD）修饰的金纳米粒子（AuNPs）涂层开管柱（OT柱）。该开管柱通过金纳米粒子在3-巯丙基三甲氧基硅烷（MPTMS）预衍生化的毛细管上自组装，随后用硫醇化β-环糊精（SH-β-CD）进行修饰而构建。采用扫描电子显微镜（SEM）、透射电子显微镜（TEM）和紫外可见光谱对制备的开管柱和合成的金纳米粒子进行表征。通过比较金纳米粒子和硫醇化β-环糊精的不同涂覆时间，得到了制备开管柱的最佳条件。此外，还对缓冲液pH值、缓冲液浓度和施加电压等分离参数进行了优化。通过分离联苯苄唑、非索非那定、奥美拉唑和兰索拉唑四对药物对映体，验证了开管柱的分离效果，对所研究的这些分析物获得了满意的分离结果。此外，该柱表现出良好的稳定性和重复性。通过日内、日间和柱间研究获得的相对标准偏差值小于5%。
