Lu Junyu, Ye Fanggui, Zhang Aizhu, Wei Zong, Peng Yan, Zhao Shulin
Key Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources (Ministry of Education of China), College of Chemistry and Chemical Engineering of Guangxi Normal University, Guilin, P. R. China.
J Sep Sci. 2011 Aug;34(16-17):2329-36. doi: 10.1002/jssc.201100102. Epub 2011 May 5.
This paper describes the development of silica monolith modified with bovine serum albumin-gold nanoparticles (BSA-GNPs) conjugates as chiral stationary phases for capillary electrochromatography (CEC). The bare monolithic silica column was prepared by a sol-gel process and has been modified chemically with 3-mercaptopropyltrimethoxysilane to provide thiol groups, followed by immobilization of gold nanoparticles via the formation of an Au-S bond and modification with BSA as the chiral selector via the nitrogen lone pair of electrons. It has been demonstrated that the monolithic chiral stationary phases can be used for the enantioseparation of a number of phenylthiocarbamyl amino acids (PTC-D/L-AAs) by CEC. Ten pairs of tested amino acids enantiomers were successfully resolved within 18 min under optimized conditions, and the resolution values were in the range of 1.486-2.083. With PTC-D/L-tryptophan used as the probe solute, the influences of applied voltage, organic modifier and buffer pH in mobile phase on apparent retention factor, enantioselectivity and resolution factor were also investigated.
本文描述了用牛血清白蛋白 - 金纳米粒子（BSA - GNPs）共轭物修饰的硅胶整体柱作为毛细管电色谱（CEC）手性固定相的开发。裸整体硅胶柱通过溶胶 - 凝胶法制备，并用3 - 巯基丙基三甲氧基硅烷进行化学修饰以提供硫醇基团，随后通过形成Au - S键固定金纳米粒子，并通过氮孤对电子用BSA作为手性选择剂进行修饰。已经证明，整体手性固定相可用于通过CEC对多种苯硫代氨基甲酰基氨基酸（PTC - D/L - AAs）进行对映体分离。在优化条件下，18分钟内成功分离了10对测试的氨基酸对映体，分离度值在1.486 - 2.083范围内。以PTC - D/L - 色氨酸作为探针溶质，还研究了流动相中施加电压、有机改性剂和缓冲液pH对表观保留因子、对映选择性和分离因子的影响。
