School of Pharmacy, China Medical University, Taichung, Taiwan.
Electrophoresis. 2010 Oct;31(19):3217-26. doi: 10.1002/elps.201000226.
A new phase containing immobilized carbon nanotubes (CNTs) was synthesized by in situ polymerization of acid-treated multi-walled CNTs using butylmethacrylate (BMA) as the monomer and ethylene dimethacrylate as the crosslinker on a silanized capillary, forming a porous-layered open-tubular column for CEC. Incorporation of CNT nanomaterials into a polymer matrix could increase the phase ratio and take advantage of the easy preparation of an OT-CEC column. The completed BMA-CNT column was characterized by SEM, ATR-IR, and EOF measurements, varying the pH and the added volume organic modifier. In the multi-walled CNTs structure, carboxylate groups were the major ionizable ligands on the phase surface exerting the EOF having electroosmotic mobility, 4.0 × 10(4) cm2 V(-1)1 S(-1)1, in the phosphate buffer at pH 2.8 and RSD values (n=5), 3.2, 4.1, and 4.3%, for three replicate capillaries at pH 7.6. Application of the BMA-CNT column in CEC separations of various samples, including nucleobases, nucleosides, flavonoids, and phenolic acids, proved satisfactory upon optimization of the running buffers. Their optima were found in the borate buffers at pH 9.0/50 mM, pH 9.5/10 mM/50% v/v ACN, and pH 9.5/30 mM/10% v/v methanol, respectively. The separations could also be used to assess the relative contributions of electrophoresis and chromatography to the CEC mechanism by calculating the corresponding velocity and retention factors. Discussions about interactions between the probe solutes and the bonded phase included the π-π interactions, electrostatic repulsion, and hydrogen bonding. Furthermore, a reversed-phase mode was discovered to be involved in the chromatographic retention.
通过在硅烷化毛细管上原位聚合酸处理的多壁 CNTs,使用甲基丙烯酸丁酯(BMA)作为单体和乙二甲基丙烯酸酯作为交联剂,合成了含有固定化 CNTs 的新相,形成了用于 CEC 的多孔层开管柱。将 CNT 纳米材料掺入聚合物基质中可以增加相比例,并利用 OT-CEC 柱的易制备性。通过 SEM、ATR-IR 和 EOF 测量对完成的 BMA-CNT 柱进行了表征,同时改变了 pH 值和添加的有机溶剂体积。在多壁 CNTs 结构中,羧酸盐是相表面上的主要可离子化配体,在 pH 2.8 的磷酸盐缓冲液中具有电渗流迁移率 4.0×10(4)cm2V(-1)1S(-1)1,在 pH 7.6 时三个重复毛细管的 RSD 值(n=5)为 3.2、4.1 和 4.3%。在 CEC 分离各种样品(包括碱基、核苷、黄酮类化合物和酚酸)的应用中,通过优化运行缓冲液证明了 BMA-CNT 柱的应用是令人满意的。它们的最佳条件分别为 pH 9.0/50 mM 硼酸盐缓冲液、pH 9.5/10 mM/50% v/v ACN 硼酸盐缓冲液和 pH 9.5/30 mM/10% v/v 甲醇硼酸盐缓冲液。通过计算相应的速度和保留因子,还可以使用分离来评估电泳和色谱对 CEC 机制的相对贡献。讨论了探针溶质与键合相之间的相互作用,包括π-π 相互作用、静电排斥和氢键。此外,还发现存在反相模式参与色谱保留。