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S-citalopram imprinted monolithic columns for capillary electrochromatography enantioseparations
Electrophoresis ( IF 2.9 ) Pub Date : 2021-08-18 , DOI: 10.1002/elps.202100222
Ali Derazshamshir 1 , Ilgım Göktürk 1 , Fatma Yılmaz 2 , Adil Denizli 1
Affiliation  

In this study, the molecular imprinting method was used to separate enantiomeric forms of chiral antidepressant drug, R,S-citalopram (R,S-CIT) in aqueous solution by CEC system combining the advantages of capillary electrophoresis (CE) and high-performance liquid chromatography (HPLC). For that, an amino acid-based molecularly imprinted monolithic capillary column was designed and used as a stationary phase for selective separation of S-citalopram (S-CIT) for the first time. S-CIT was selectively separated from the aqueous solution containing the other enantiomeric form of R-CIT, which is the same in size and shape as the template molecule. Morphology of the molecularly imprinted (MIP S-CIT) and non-imprinted (NIP S-CIT) monolithic capillary columns was observed by scanning electron microscopy. Imprinting efficiency of MIP S-CIT monolithic capillary column used for selective S-CIT separation was verified by comparing with NIP S-CIT and calculated imprinting factor (I.F:1.81) proved the high selectivity of the MIP S-CIT for S-CIT. Cavities formed for S-CIT form enabled selective (α = 2.08) separation of the target molecule from the other enantiomeric R-CIT form. Separation was achieved in a short period of 10 min, with the electrophoretic mobility of 7.68 × 10−6 m2/Vs for R,S-CIT at pH 7.0 10 mM PB and 50% ACN ratio. The performance of both MIP S-CIT and NIP S-CIT columns was estimated by repeating the R,S-CIT separations with intra-batch and inter-batch studies for reproducibility of retention times of R,S-CITs. Estimated RSD values that are lower than 2% suggest that the monolithic columns separate R,S-CIT enantiomers without losing separation efficiency.

中文翻译:

用于毛细管电色谱对映体分离的 S-西酞普兰印迹整体柱

本研究采用分子印迹法,结合毛细管电泳 (CE) 和高效能的优点,通过 CEC 系统分离水溶液中手性抗抑郁药物 R,S-西酞普兰 (R,S-CIT) 的对映体形式。液相色谱法(HPLC)。为此,首次设计了基于氨基酸的分子印迹整体式毛细管柱,并将其作为固定相用于选择性分离S-西酞普兰(S-CIT)。S-CIT 从含有另一种对映体形式的 R-CIT 的水溶液中选择性地分离出来,它的大小和形状与模板分子相同。通过扫描电子显微镜观察分子印迹 (MIP S-CIT) 和非印迹 (NIP S-CIT) 整体毛细管柱的形态。通过与NIP S-CIT的比较验证了用于选择性分离S-CIT的MIP S-CIT整体毛细管柱的印迹效率,计算的印迹因子(IF:1.81)证明了MIP S-CIT对S-CIT的高选择性。为 S-CIT 形式形成的空腔启用了选择性 (α = 2.08) 目标分子与其他对映体 R-CIT 形式的分离。在 10 分钟的短时间内实现分离,R,S-CIT 在 pH 7.0 10 mM PB 和 50% ACN 比率下的电泳迁移率为 7.68 × 10 -6 m 2 /Vs。MIP S-CIT 和 NIP S-CIT 色谱柱的性能通过重复 R,S-CIT 分离以及批次内和批次间研究来评估 R,S-CIT 保留时间的重现性。低于 2% 的估计 RSD 值表明整体柱分离 R,S-CIT 对映异构体而不会损失分离效率。
更新日期:2021-08-18
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