Key Laboratory of Drug Quality Control and Pharmacovigilance (Ministry of Education), China Pharmaceutical University, Nanjing 210009, PR China; State Key Laboratory of Natural Medicines, China Pharmaceutical University, Nanjing 210009, PR China.
Key Laboratory of Drug Quality Control and Pharmacovigilance (Ministry of Education), China Pharmaceutical University, Nanjing 210009, PR China; State Key Laboratory of Natural Medicines, China Pharmaceutical University, Nanjing 210009, PR China.
J Pharm Biomed Anal. 2022 Jun 5;215:114777. doi: 10.1016/j.jpba.2022.114777. Epub 2022 Apr 19.
Metal organic frameworks (MOFs), as a novel separation mediums, have in recent years attracted wide consideration in capillary electrochromatography (CEC). However, the instability of frameworks limited the application of the MOF-based chiral separation capillary. Herein, Iron-based γ-cyclodextrin metal-organic framework (Fe-CD-MOF) with mesoporous was developed as the chiral stationary phase in open tubular capillary electrochromatography column (OT-CEC) for the stereoisomer separation of fourteen chiral drugs and one chiral alcohol. The capillary column with MOF coating exhibited the best performance (resolution value: 17.07) for anisodamine in any MOF-based capillary column that has never been reported. Moreover, the effect of pH, buffer concentration, and methanol content has been investigated. The novel coated capillary was also applied for the quantitative analysis of a real sample. The Fe-CD-MOF coated capillary showed outstanding repeatability and stability, with the satisfactory relative standard deviations (RSDs) for intra-day, inter-day, and column-to-column. Finally, the enantioseparation mechanism of the Fe-CD-MOF coated capillary was evaluated by adsorption kinetic experiments. In summary, this work indicated the novel and renewable Fe-CD-MOF was a potential chiral stationary phase in CEC chiral separation.
金属有机骨架（MOFs）作为一种新型的分离介质，近年来在毛细管电色谱（CEC）中引起了广泛的关注。然而，MOFs 的不稳定性限制了基于 MOF 的手性分离毛细管的应用。本文以介孔γ-环糊精金属有机骨架（Fe-CD-MOF）为手性固定相，制备了开放式管状毛细管电色谱柱（OT-CEC），用于 14 种手性药物和 1 种手性醇的对映异构体分离。在任何基于 MOF 的毛细管柱中，涂覆 MOF 的毛细管柱对手性药物山莨菪碱的分离性能最佳（分辨率值：17.07），这是以前从未报道过的。此外，还考察了 pH 值、缓冲液浓度和甲醇含量的影响。该新型涂覆毛细管还用于实际样品的定量分析。Fe-CD-MOF 涂覆毛细管显示出出色的重现性和稳定性，日内、日间和柱间的相对标准偏差（RSD）均令人满意。最后，通过吸附动力学实验评价了 Fe-CD-MOF 涂覆毛细管的手性分离机制。综上所述，本研究表明新型可再生 Fe-CD-MOF 是 CEC 手性分离中一种有潜力的手性固定相。
