School of Chemistry and Environment, South China Normal University, Guangzhou, P. R. China.
School of Logistics, Beijing Normal University, Zhuhai Campus, Zhuhai, P. R. China.
Electrophoresis. 2018 Jan;39(2):348-355. doi: 10.1002/elps.201700273. Epub 2017 Nov 10.
A new single-urea-bound chiral stationary phase based on 3,5-dimethylphenylcarbamoylated β-cyclodextrin was prepared through the Staudinger reaction of mono (6 -azido-6 -deoxy)-per(3,5-dimethylphenylcarbamoylated) β-cyclodextrin and 3-aminopropyl silica gel under CO atmosphere. The new phase exhibited good enantioseparation performance for 33 analytes using normal-phase HPLC conditions; 19 of them were baseline separated. Effects of structure of analytes, alcoholic modifiers, and acidic/basic additives on separation performances of this new cyclodextrin chiral stationary phase have been studied in detail. The results showed that the retention and resolution of acidic and basic analytes on the CSP were greatly affected by the additives. Peak symmetry for some analytes could be improved by simultaneously adding acidic and basic additives to the mobile phase. This work expands the potential applications of the cyclodextrin-based chiral stationary phases in the normal-phase HPLC.
一种基于 3,5-二甲基苯甲酰化 β-环糊精的新型单脲键手性固定相,通过单(6-叠氮-6-脱氧)-全(3,5-二甲基苯甲酰化)β-环糊精与 3-氨丙基硅胶在 CO 气氛下的 Staudinger 反应制备。该新相在正相 HPLC 条件下对 33 种分析物表现出良好的对映体分离性能;其中 19 种可实现基线分离。详细研究了分析物结构、醇改性剂和酸碱添加剂对该新型环糊精手性固定相分离性能的影响。结果表明,添加剂对酸性和碱性分析物在 CSP 上的保留和分离度有很大影响。通过同时向流动相中添加酸性和碱性添加剂,可以改善某些分析物的峰形对称性。这项工作扩展了基于环糊精的手性固定相在正相 HPLC 中的潜在应用。