Layer-by-layer self-assembly of gold nanoparticles/thiols β-cyclodextrin coating as the stationary phase for enhanced chiral differentiation in open tubular capillary electrochromatography
Layer-by-layer self-assembly of gold nanoparticles/thiols β-cyclodextrin coating as the stationary phase for enhanced chiral differentiation in open tubular capillary electrochromatography
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DOI：
10.1016/j.talanta.2017.01.082
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发表时间：
2017-05-15
期刊：
影响因子：
6.1
通讯作者：
Guo, Xing-jie
中科院分区：
文献类型：
--
作者：
Fang, Lin-lin;Wang, Ping;Guo, Xing-jie
毛细管电色谱（CEC）的发展和应用，使得对映体选择性CEC体系的研究越来越多。本文首次报道了一种新的、简单、经济的制备对映体选择性开管毛细管电色谱手性固定相的方法。这种新型毛细管柱是通过层层自组装的GNP在3-巯丙基三甲氧基硅烷（MPTMS）改性的熔融石英毛细管和随后的表面功能化的GNP通过硫醇β-环糊精（SH-β-CD）的自组装。以美普他酚及其三种中间体为模板，制备了单层和多层GNP膜毛细管柱，并对其性能进行了评价。因此，三层GNP毛细管柱表现出良好的对映体分离性能。考察了影响手性分离度的因素。在优化的条件下，美普他酚及其三个中间体（中间体II、III和IV）在20 min内得到了对映选择性，分离度分别为2.05、0.36、1.67和1.53。拟定色谱柱显示了运行间和日常的充分重复性。总之，这些结果证实了使用GNP作为电色谱载体可以提高毛细管电色谱（CEC）中OTC柱的相比。该方法具有良好的线性（10.999）、回收率（92.0-94.5%）和重复性，并成功地用于尿样中美普他酚的对映体分离，表明该柱在生物分析中具有潜在的应用价值。
The popularity of capillary electrochromatography (CEC) has led to an increasing number of studies on the development and evaluation of enantioselective CEC systems. Herein, a novel, simple, and economical method for the preparation of chiral stationary phases for enantioselective open tubular capillary electrochromatography (OTCEC) was reported for the first time. This novel capillary column was fabricated through layer-by layer self-assembly of GNPs on a 3-mercaptopropyl-trimethoxysilane (MPTMS)-modified fused-silica capillary and subsequent surface functionalization of the GNPs through self-assembly of thiols beta-cyclodextrin (SH-beta-CD). With this method, monolayer and multilayer GNPs film capillary columns were prepared and evaluated using meptazinol and its three intermediate enantiomers as templates. Consequently, the three-layer GNPs capillary column was found to exhibit favorable enantioseparation performance. Factors that influence the chiral separation resolution were examined. Under the optimized conditions, enantioselectivity was obtained for meptazinol and its three intermediate enantiomers (intermediates II, III and IV) in less than 20 min with resolutions of 2.05, 0.36, 1.67, 1.53, respectively. The proposed column revealed adequate repeatability concerning run-to-run and day-to-day. In brief, these results confirmed the use of GNPs as the electro-chromatographic support can enhance the phase ratio of OTC column in capillary electrochromatography (CEC). Then, this proposed method was well validated with good linearity (10.999), recovery (92.0-94.5%) and repeatability, and was successfully used for enantioseparation of meptazinol in spiked urine samples, which indicated the new column's potential usage in biological analysis.