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手性拆分能力的比较研究直链淀粉三(3-氯-5-甲基苯基氨基甲酸酯)键合硅胶在纳流液相色谱和毛细管电色谱中的应用。

Comparative study on enantiomer resolving ability of amylose tris(3-chloro-5-methylphenylcarbamate) covalently immobilized onto silica in nano-liquid chromatography and capillary electrochromatography.

机构信息

Istituto per i Sistemi Biologici (ISB), CNR- Consiglio Nazionale delle Ricerche, Via Salaria Km 29, 300 - 00015, Monterotondo, Rome, Italy.

Department of Medicine, University Campus Bio-Medico of Rome, Via Alvaro del Portillo 21, 00128, Rome, Italy.

出版信息

J Chromatogr A. 2019 Nov 22;1606:460425. doi: 10.1016/j.chroma.2019.460425. Epub 2019 Aug 12.

Abstract

In the present study separation of enantiomers of some chiral neutral and weakly acidic analytes was investigated on the chiral stationary phase (CSP) made by covalent immobilization of amylose tris(3-chloro-5-methylphenylcarbamate) onto silica in nano-liquid chromatography (nano-LC) and capillary electrochromatography (CEC) in acetonitrile and aqueous acetonitrile. Few comparisons were made also between the enantioseparations in nano-LC and high-performance liquid chromatography (HPLC) with the chiral column of 4.6 × 250 mm dimension. Slightly better separation of enantiomers was observed in HPLC mode compared to nano-LC mode. It was shown that in the capillary columns packed with the CSP containing about 20% (w/w) of a covalently immobilized neutral chiral selector, amylose tris(3-chloro-5-methylphenylcarbamate), sufficient electroosmotic flow has been generated and enantioseparations with reasonable analysis time were performed also in CEC mode. It was shown once again that CEC offers a clear advantage over nano-LC from the viewpoint of plate numbers and peak resolution.

摘要

在本研究中,通过将直链淀粉三(3-氯-5-甲基苯基氨基甲酸酯)共价固定到硅胶上,在纳米液相色谱(nano-LC)和在乙腈和含水乙腈中的胶束电动色谱(CEC)中研究了一些手性中性和弱酸性分析物对映体的分离。还比较了在 nano-LC 和高效液相色谱(HPLC)中使用 4.6×250mm 尺寸的手性柱时的对映体分离。与 nano-LC 模式相比,HPLC 模式对手映体的分离稍好。结果表明,在填充有约 20%(w/w)共价固定的中性手性选择剂直链淀粉三(3-氯-5-甲基苯基氨基甲酸酯)的毛细管柱中,已产生足够的电动流,并且也可以在 CEC 模式下以合理的分析时间进行对映体分离。再次表明,从塔板数和峰分辨率的角度来看,CEC 比 nano-LC 具有明显的优势。

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