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Enantiomeric separation of some chiral analytes using amylose 3,5-dimethylphenylcarbamate covalently immobilized on silica by nano-liquid chromatography and capillary electrochromatography
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2017-09-08 , DOI: 10.1016/j.chroma.2017.09.017
Giovanni D’Orazio , Chiara Fanali , Marina Karchkhadze , Bezhan Chankvetadze , Salvatore Fanali

A new experimental chiral stationary phase containing amylose 3,5-dimethylphenylcarbamate immobilized onto silica gel (i-ADMPC) was packed in 100 μm I.D. fused silica capillary and used for the chiral separation of eight selected flavanone derivatives in polar organic mobile phase by using different miniaturized techniques, such as nano-liquid chromatography (nano-LC), capillary electrochromatography (CEC) and pressure-assisted CEC (pCEC). A comparative study of different elution modes in terms of chromatographic efficiency, analysis time and enantiomeric resolution was carried out. In pCEC mode, the highest chromatography performance was obtained applying +2.5 kV voltage and inlet pressure 10 bar. Under these conditions, the analysis times were shorter than 20 min, and chromatographic efficiencies were in the range 33,000–49,000 plates/m (first eluted peak).

The solvent versatility of packed i- ADMPC capillary column was also investigated. In nano-LC, the CSP was stressed under the use of strong organic solvents such as ethyl acetate, acetone and methyl t-butyl ether (MTBE). After at least 40 working hours and over 50 sample injections, the CSP resulted to be very stable allowing to achieve good repeatability employing again the mobile phase containing polar organic solvent. Enantioresolutions and chromatographic efficiencies decreased by 1.60 and 10%, respectively as the result of using above mentioned strong solvents.



中文翻译:

使用纳米液相色谱和毛细管电色谱法共价固定在硅胶上的直链淀粉3,5-二甲基苯基氨基甲酸酯对映异构体分离某些手性分析物

将固定在硅胶上的含有3,5-二甲基苯基氨基甲酸直链淀粉的新型实验手性固定相装入100μmID熔融石英毛细管中,并通过使用不同的手性方法在极性有机流动相中手性分离出八种选定的黄烷酮衍生物。小型化技术,例如纳米液相色谱(nano-LC),毛细管电色谱(CEC)和压力辅助CEC(pCEC)。对不同洗脱方式的色谱效率,分析时间和对映体分离度进行了比较研究。在pCEC模式下,使用+2.5 kV电压和10 bar的入口压力可获得最高的色谱性能。在这些条件下,分析时间短于20分钟,色谱效率在33,000–49之间,

还研究了填充式i- ADMPC毛细管柱的溶剂通用性。在nano-LC中,CSP在使用强有机溶剂(如乙酸乙酯,丙酮和甲基叔丁基醚(MTBE))的作用下受到压力。经过至少40个工作小时和超过50次进样后,CSP变得非常稳定,再次使用含有极性有机溶剂的流动相即可实现良好的重复性。由于使用了上述强溶剂,对映体分离度和色谱效率分别降低了1.60和10%。

更新日期:2017-09-08
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