School of Chemical Technology, Liaoning & Shenyang Key Laboratory of Functional Dye and Pigment, Shenyang University of Chemical Technology, Shenyang, P. R. China.
Mikrochim Acta. 2024 Jul 9;191(8):457. doi: 10.1007/s00604-024-06533-8.
A new enantioselective open-tubular capillary electrochromatography (OT-CEC) was developed employing β-cyclodextrin covalent organic frameworks (β-CD COFs) conjugated gold-poly glycidyl methacrylate nanoparticles (Au-PGMA NPs) as a stationary phase. The resulting coating layer on the inner wall of the fabricated capillary column was characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), energy dispersive spectroscopy (EDS), and electroosmotic flow (EOF) experiments. The performance of the fabricated capillary column was evaluated by CEC using enantiomers of seven model analytes, including two proton pump inhibitors (PPIs, omeprazole and tenatoprazole), three amino acids (AAs, tyrosine, phenylalanine, and tryptophan), and two fluoroquinolones (FQs, gatifloxacin and sparfloxacin). The influences of coating time, buffer concentration, buffer pH, and applied voltage on enantioseparation were investigated to obtain satisfactory enantioselectivity. In the optimum conditions, the enantiomers of seven analytes were fully resolved within 10 min with high resolutions of 3.03 to 5.25. The inter- to intra-day and column-to-column repeatabilities of the fabricated capillary column were lower than 4.26% RSD. Furthermore, molecular docking studies were performed based on the chiral fabricated column and as ligand isomers of analytes using Auto Dock Tools. The binding energies and interactions acquired from docking results of analytes supported the experimental data.
一种新的手性开管毛细管电色谱(OT-CEC)采用β-环糊精共价有机骨架(β-CD COFs)键合金-聚缩水甘油甲基丙烯酸酯纳米粒子(Au-PGMA NPs)作为固定相。通过扫描电子显微镜(SEM)、傅里叶变换红外光谱(FT-IR)、能谱(EDS)和电渗流(EOF)实验对制备的毛细管柱内壁上的涂层进行了表征。通过使用七种模型分析物的对映异构体进行 CEC 评价了制备的毛细管柱的性能,包括两种质子泵抑制剂(PPIs,奥美拉唑和替那拉唑)、三种氨基酸(AA,酪氨酸、苯丙氨酸和色氨酸)和两种氟喹诺酮类药物(FQs,加替沙星和司帕沙星)。考察了涂层时间、缓冲液浓度、缓冲液 pH 值和施加电压对映异构体分离的影响,以获得满意的对映选择性。在最佳条件下,七种分析物的对映异构体在 10 分钟内完全分离,分辨率为 3.03 至 5.25。制备的毛细管柱的日内和柱间重复性低于 4.26%RSD。此外,根据手性制备柱和作为分析物配体异构体的 Auto Dock Tools 进行了分子对接研究。对接结果中分析物的结合能和相互作用支持实验数据。