Ma Y, Ito Y
Laboratory of Biophysical Chemistry, National Heart, Lung, and Blood Institute, National Institutes of Health, Bethesda, Maryland 20892-1676, USA.
Anal Chem. 1995 Sep 1;67(17):3069-74. doi: 10.1021/ac00113a049.
Various parameters involved in the chiral separation of (+/-)-DNB-amino acids were investigated using N-dodecanoyl-L-proline-3,5-dimethylanilide as a chiral selector (CS) and two-phase solvent systems composed of hexane/ethyl acetate/methanol/10 mM hydrochloric acid at various volume ratios. The results indicated that increasing the concentration or net amount of the CS in the stationary phase improves both separation factor (alpha) and peak resolution (Rs). The hydrophobicity of the solvent system also increases the alpha value of the racemate while it affects the peak resolution differently according to the partition coefficient of the racemate. Overall results indicated that the best separation of a racemate will be achieved by applying a high CS concentration in the organic phase while adjusting the hydrophobicity of the solvent system so that the partition coefficient of the racemate falls between 0.6 and 0.8. The peak resolution will be further increased by using a longer and/or greater internal diameter coiled column.
使用N-十二烷酰-L-脯氨酸-3,5-二甲基苯胺作为手性选择剂（CS）以及由己烷/乙酸乙酯/甲醇/10 mM盐酸按不同体积比组成的两相溶剂体系，研究了(±)-DNB-氨基酸手性分离过程中涉及的各种参数。结果表明，增加固定相中CS的浓度或净含量可提高分离因子（α）和峰分辨率（Rs）。溶剂体系的疏水性也会增加外消旋体的α值，同时根据外消旋体的分配系数对峰分辨率产生不同影响。总体结果表明，通过在有机相中应用高浓度的CS，同时调节溶剂体系的疏水性以使外消旋体的分配系数落在0.6至0.8之间，可实现外消旋体的最佳分离。使用更长和/或更大内径的盘管柱可进一步提高峰分辨率。
