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瞬态滞留-环糊精电动色谱法的灵敏对映体分离。

Sensitive enantioseparation by transient trapping-cyclodextrin electrokinetic chromatography.

机构信息

Department of Material Chemistry, Graduate School of Engineering, Kyoto University, Katsura, Nishikyo-ku, Kyoto 615-8510, Japan.

出版信息

J Chromatogr A. 2012 Dec 21;1269:366-71. doi: 10.1016/j.chroma.2012.08.065. Epub 2012 Aug 27.

Abstract

An on-line sample preconcentration based on transient trapping was applied to cyclodextrin electrokinetic chromatography (CDEKC) to realize a highly sensitive chiral analysis in capillary electrophoresis. The partial introduction of a micellar solution before the electrokinetic injection of a sample solution provided the effective preconcentration and enantioseparation of chiral compounds, resulting in the up to 240-fold enhancements of peak intensity and 100-fold improvements of limit of detection of (R),(S)-1-aminoindan as the model analyte. The demonstrated method could be applied to the other pharmaceutical compounds, which allowed five chiral analytes to be resolved with 40- to 160-fold sensitivity enhancements at once. The enantioseparation efficiency of the proposed method was slightly lower as compared to the conventional CDEKC, while the acceptable baseline separations of enantiomers were obtained in transient trapping-CDEKC relative to the undesirable resolution in the CDEKC with other preconcentration techniques. Additionally, it was clarified that transient trapping-CDEKC was also applicable to the analysis of enantiomeric excess, providing the sensitive detection of 43ppb of (R)-chlorpheniramine in 5ppm (S)-chlorpheniramine solution commercially available.

摘要

基于瞬态捕集的在线样品预浓缩被应用于环糊精电动色谱(CDEKC)中,以在毛细管电泳中实现高灵敏度的手性分析。在电动力学进样样品溶液之前部分引入胶束溶液,为手性化合物的有效预浓缩和对映体分离提供了条件,从而使(R),(S)-1-氨基茚满作为模型分析物的峰强度提高了 240 倍,检测限提高了 100 倍。所展示的方法可以应用于其他药物化合物,一次可以同时实现 5 种手性分析物的分离,灵敏度提高了 40 到 160 倍。与其他预浓缩技术相比,与传统 CDEKC 相比,该方法的对映体分离效率略低,但在瞬态捕集-CDEKC 中可以获得可接受的对映体基线分离,而在 CDEKC 中使用其他预浓缩技术则无法实现。此外,还阐明了瞬态捕集-CDEKC 也适用于对映体过量的分析,能够在市售的 5ppm(S)-氯苯那敏溶液中检测到 43ppb 的(R)-氯苯那敏。

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