α-氨基膦酸酯类化合物在直链淀粉手性固定相上的高效液相色谱分离
Enantioseparation of Novel α-Aminophosphonate Esters on the Amylose Derivative Chiral Stationary Phases by HPLC
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摘要: 采用直链淀粉-三(3,5-二甲基苯基氨基甲酸酯)键合型手性固定相(Chiralpak IA柱)和涂敷型手性固定相(Chiralpak AD-H柱)对6个O,O'-二烷基-α-(氟代苯乙基)氨基-3,4,5-三甲氧基苯基甲基膦酸酯化合物进行了直接手性拆分研究,在正己烷/异丙醇、正己烷/乙醇两种不同流动相条件下,6个化合物均能在AD-H柱上实现基线分离,AD-H柱的手性分离效果优于IA柱。并考察了AD-H柱在以正己烷/乙醇作流动相时,不同温度及乙醇浓度对手性分离的影响。结果表明,在10 ~40℃范围内随着温度的降低,化合物的分离因子、分离度均增大,在乙醇体积分数为5% ~15%范围内,随乙醇浓度的降低,化合物的分离度增大,分离因子基本保持不变。表明AD-H柱可推荐用于此类化合物的半制备手性分离。Abstract: The direct HPLC enantioseparation of six O,O'-dialkyl-α-(fluorinated phenylethy1)amino-3,4,5-trimethoxybenzy1 methy1 phosphonates on coated and immobilized amylose tris-(3,5-dimethyphenylcarbamate) chiral stationary phases (Chiralpak AD-H and Chiralpak IA) was presented.In n-hexane/2-isopropanol and n-hexane/ethanol mixtures,all studied compounds can be baseline separated on AD-H column,AD-H column exhibits better separation effect for all compounds than IA column.The effect of temperature and ethanol organic modifier concentration on the resolution was investigated on AD-H column.The results showed in the range of 10 ~40℃,resolution factors and sepatation factors increased with decreasing temperature; in the range of 5% ~15% ethanol in n-hexane,resolution factors increase with decreasing solvent polarity and separation factors were relatively stable.AD-H was recommended to carry out chiral semi-preparative separation of all compounds.
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