Aranyi Anita, Ilisz István, Péter Antal, Fülöp Ferenc, West Caroline
Department of Inorganic and Analytical Chemistry, University of Szeged, Dóm tér 7, H-6720 Szeged, Hungary; University of Orleans, Institute of Organic and Analytical Chemistry (ICOA) , CNRS UMR 7311, Pôle de Chimie, rue de Chartres, 45067 Orleans Cedex 2, France.
Department of Inorganic and Analytical Chemistry, University of Szeged, Dóm tér 7, H-6720 Szeged, Hungary.
J Chromatogr A. 2015 Mar 27;1387:123-33. doi: 10.1016/j.chroma.2015.01.084. Epub 2015 Feb 7.
The direct separation of the enantiomers of 1-(α-aminoarylmethyl)-2-naphthol, 1-(α-aminoalkyl)-2-naphthol, 2-(α-aminoarylmethyl)-1-naphthol analogues and 2-(1-amino-2-methylpropyl)-1-naphthol) was investigated in supercritical fluid chromatography. Five commercially available chiral stationary phases based on immobilized polysaccharide chiral selectors (Chiralpak IA, IB, IC, ID and IE) were evaluated. Chiralpak IB was by far the most efficient to achieve the separation of these racemates and was further selected for optimization of elution conditions. The effects of column temperature (varying between 5 and 45 °C) and co-solvent added to carbon dioxide (methanol, ethanol, isopropanol and dichloromethane) were investigated. A particular attention was paid to mobile-phase additives. Several of them, acids, bases or salts (namely water, formic acid, acetic acid, trifluoroacetic acid, diethylamine, diethanolamine, triethylamine, triethanolamine, dimethylethanolamine, ammonia and ammonium acetate), were tested in order to improve peak shapes while maintaining selectivity. With the help of other achiral naphthol derivatives, the additive effects were examined.
在超临界流体色谱法中研究了1-(α-氨基芳基甲基)-2-萘酚、1-(α-氨基烷基)-2-萘酚、2-(α-氨基芳基甲基)-1-萘酚类似物和2-(1-氨基-2-甲基丙基)-1-萘酚对映体的直接分离。评估了五种基于固定化多糖手性选择剂的市售手性固定相(Chiralpak IA、IB、IC、ID和IE)。到目前为止,Chiralpak IB在分离这些外消旋体方面效率最高,并进一步被选用于优化洗脱条件。研究了柱温(在5至45°C之间变化)和添加到二氧化碳中的共溶剂(甲醇、乙醇、异丙醇和二氯甲烷)的影响。特别关注流动相添加剂。测试了其中几种,酸、碱或盐(即水、甲酸、乙酸、三氟乙酸、二乙胺、二乙醇胺、三乙胺、三乙醇胺、二甲基乙醇胺、氨和乙酸铵),以便在保持选择性的同时改善峰形。借助其他非手性萘酚衍生物,研究了添加剂的效果。