探索纤维素三-3,5-二氯苯基氨基甲酸酯作为手性电色谱法分离唑类抗真菌药的固定相的性能

Massimo Giuseppe De Cesaris , Giovanni D'Orazio , Chiara Fanali , Alessandra Gentili , Salvatore Fanali
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引用次数: 0

摘要

本研究考察了纤维素三-3,5-二氯苯基氨基甲酸酯(CDCPC)作为手性选择剂对一些手性抗真菌化合物进行对映体分离时的对映体识别和分离性能。采用 "浆液法 "将 CDCPC 与 5 µm 多孔硅胶颗粒结合,并将固定相填入熔融石英毛细管(内径为 250 mm x 75 µm)。该色谱柱用于通过毛细管电色谱法(CEC)分离十二种选定的唑类化合物的对映体。为了研究手性识别,改变了流动相的有机溶剂、水含量、缓冲剂类型、浓度和 pH 值。每种改变都会增强特定的相互作用,从而导致手性识别。本文对这些变化对保留因子、对映体解析度和峰展宽的影响进行了深入探讨。所开发的方法被用作评估固定相在不同流动相条件下稳定性的适当测试台,即使在连续使用几十个小时后,也能显示出显著的对映选择能力。优化后的 CEC-UV 方法对 12 种唑类杀菌剂中 7 种杀菌剂的对映体分离非常有效,在一次 30 分钟的运行分析中总共分离出 14 个峰。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

Exploring the performance of cellulose tris-3,5-dichlorophenylcarbamate as a stationary phase for the chiral electro-chromatographic separation of azole antifungals

Exploring the performance of cellulose tris-3,5-dichlorophenylcarbamate as a stationary phase for the chiral electro-chromatographic separation of azole antifungals

In this study, the enantiorecognition and separation performance of cellulose tris-3,5-dichlorophenylcarbamate (CDCPC) as the chiral selector for the enantioseparation of some chiral antifungal compounds was investigated. The CDCPC was bonded to 5 µm porous silica particles and the stationary phase packed into fused silica capillaries (250 mm x 75 µm I.D.) using the "slurry method". The column was used for the separation of twelve selected azole compounds in their enantiomers by capillary electrochromatography (CEC). To study chiral recognition, the mobile phase was modified changing the organic solvent, water content, buffer type, concentration, and pH. Each change resulted in the enhancement of specific interactions at the expense of others, leading to chiral recognition. Their effects on retention factors, enantiomeric resolution, and peak broadening are critically discussed. The developed methodology was used as an appropriate test bench to evaluate the stability of the stationary phase under different mobile phase conditions, demonstrating a remarkable enantioselective capacity even after several tens of hours of continuous use. The optimized CEC-UV method was very effective in the enantiomeric separation of seven out of twelve azole fungicides, totaling fourteen separated peaks in a single 30 min run analysis.

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来源期刊
Journal of chromatography open
Journal of chromatography open Analytical Chemistry
CiteScore
2.50
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