CHIRAL SEPARATION BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY

CHIRAL SEPARATION BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY
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DOI:
10.1021/ac00113a049
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发表时间:
1995-09-01
影响因子:
7.4
通讯作者:
ITO, Y
ITO, Y
中科院分区:
化学1区
文献类型:
--
作者:
MA, Y;ITO, Y

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以N-十二烷酰基-L-脯氨酸-3,5-二甲基苯胺为手性选择剂,在正己烷/乙酸乙酯/甲醇/10 mM盐酸(体积比)的两相溶剂体系中,考察了(+/-)-DNB-氨基酸的手性分离的各种参数。结果表明,增加固定相中CS的浓度或净含量可改善分离因子(α)和峰分辨率(R(s))。溶剂系统的疏水性也增加了外消旋体的α值,同时根据外消旋体的分配系数,其对峰分辨率的影响不同。总体结果表明,通过在有机相中应用高CS浓度同时调节溶剂系统的疏水性使得外消旋体的分配系数福尔斯落在0.6和0.8之间,将实现外消旋体的最佳分离。通过使用更长和/或更大内径的盘绕柱,将进一步提高峰分离度。
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 (R(s)). 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.