D'Orazio Giovanni, Fanali Chiara, Karchkhadze Marina, Chankvetadze Bezhan, Fanali Salvatore
Institute of Chemical Methodologies, Italian National Research Council, 00015 Monterotondo, Italy.
Centro Integrato di Ricerca, Campus Bio-Medico University, Rome, Italy.
J Chromatogr A. 2017 Oct 20;1520:127-134. doi: 10.1016/j.chroma.2017.09.017. Epub 2017 Sep 8.
A new experimental chiral stationary phase containing amylose 3,5-dimethylphenylcarbamate immobilized onto silica gel (i-ADMPC) was packed in 100μm 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 +2.5kV voltage and inlet pressure 10bar. Under these conditions, the analysis times were shorter than 20min, 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.
一种新型实验性手性固定相，其为负载于硅胶上的直链淀粉3,5 - 二甲基苯基氨基甲酸酯（i - ADMPC），被装填于内径100μm的熔融石英毛细管中，并通过使用不同的微型化技术，如纳米液相色谱（nano - LC）、毛细管电色谱（CEC）和压力辅助毛细管电色谱（pCEC），用于在极性有机流动相中对八种选定的黄烷酮衍生物进行手性分离。开展了关于不同洗脱模式在色谱效率、分析时间和对映体分离度方面的比较研究。在pCEC模式下，施加 +2.5kV电压和入口压力10bar时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 - 49,000塔板数/米（第一个洗脱峰）范围内。还研究了装填的i - ADMPC毛细管柱的溶剂通用性。在nano - LC中，使用乙酸乙酯、丙酮和甲基叔丁基醚（MTBE）等强有机溶剂时，手性固定相受到压力。在至少40个工作小时和超过50次进样后，手性固定相表现出非常稳定的性能，再次使用含极性有机溶剂的流动相时可实现良好的重复性。由于使用上述强溶剂，对映体分离度和色谱效率分别下降了1.60%和10%。
