Liu Yikun, He Ning, Lu Yingfang, Li Weiqiang, He Xin, Li Zhentao, Chen Zilin
Department of Orthopedics Trauma and Microsurgery, Zhongnan Hospital of Wuhan University, School of Pharmaceutical Sciences, Wuhan University, Wuhan, 430072, China.
Key Laboratory of Combinatorial Biosynthesis and Drug Discovery, Ministry of Education, Hubei Province Engineering and Technology Research Center for Fluorinated Pharmaceuticals, Wuhan, 430071, China.
J Pharm Anal. 2023 Feb;13(2):209-215. doi: 10.1016/j.jpha.2022.10.006. Epub 2022 Nov 2.
Here, a styrene-based polymer monolithic column poly(VBS--TAT--AHM) with reversed-phase/hydrophilic interaction liquid chromatography (RPLC/HILIC) bifunctional separation mode was successfully prepared for capillary electrochromatography by the in situ polymerization of sodium p-styrene sulfonate (VBS) with cross-linkers 3-(acryloyloxy)-2-hydroxypropyl methacrylate (AHM) and 1,3,5-triacryloylhexahydro-1,3,5-triazine (TAT). The preparation conditions of the monolith were optimized. The morphology and formation of the poly(VBS--TAT--AHM) monolith were confirmed by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR). The separation performances of the monolith were evaluated systematically. It should be noted that the incorporation of VBS functional monomer can provide π-π interactions, hydrophilic interactions, and ion-exchange interactions. Hence, the prepared poly(VBS--TAT--AHM) monolith can achieve efficient separation of thiourea compounds, benzene series, phenol compounds, aniline compounds and sulfonamides in RPLC or HILIC separation mode. The largest theoretical plate number for ,-dimethylthiourea reached 1.7 × 10 plates/m. In addition, the poly(VBS--TAT--AHM) monolithic column showed excellent reproducibility and stability. This novel monolithic column has great application value and potential in capillary electrochromatography (CEC).
在此，通过对苯乙烯磺酸钠（VBS）与交联剂甲基丙烯酸3-（丙烯酰氧基）-2-羟丙酯（AHM）和1,3,5-三丙烯酰基六氢-1,3,5-三嗪（TAT）进行原位聚合，成功制备了一种具有反相/亲水作用液相色谱（RPLC/HILIC）双功能分离模式的苯乙烯基聚合物整体柱用于毛细管电色谱。对整体柱的制备条件进行了优化。通过扫描电子显微镜（SEM）和傅里叶变换红外光谱（FT-IR）对聚（VBS-TAT-AHM）整体柱的形态和形成进行了确认。系统评价了整体柱的分离性能。需要注意的是，VBS功能单体的引入可提供π-π相互作用、亲水相互作用和离子交换相互作用。因此，制备的聚（VBS-TAT-AHM）整体柱能够在RPLC或HILIC分离模式下实现对硫脲类化合物、苯系物、酚类化合物、苯胺类化合物和磺酰胺类化合物的高效分离。对二甲硫脲的最大理论塔板数达到1.7×10⁴块/m。此外，聚（VBS-TAT-AHM）整体柱表现出优异的重现性和稳定性。这种新型整体柱在毛细管电色谱（CEC）中具有很大的应用价值和潜力。
