Caccamese Salvatore, Bianca Salvatore, Carter Guy T
Dipartimento di Scienze Chimiche, Università di Catania, Viale A. Doria 6, Catania, Italy.
Chirality. 2007 Aug;19(8):647-53. doi: 10.1002/chir.20438.
The HPLC enantiomeric separation of N-benzyl-alpha-methyl-benzylamine, phenylalaninol, tryptophanol, 2 (diphenylhydroxymethyl)pyrrolidine, and isoproterenol was accomplished in the normal-phase mode using two polysaccharide-derived chiral stationary phases (CSPs) and various n-hexane/2-propanol mobile phases with acidic (TFA) or basic (DEA) additive. The compounds were separated without any derivatization and separation factor range between 2.09 and 1.09 with resolution factor 3.4 and 0.4, respectively. The best separation of the enantiomers of the amine was achieved on amylose tris (3, 5-dimethylphenylcarbamate) CSP with TFA additive in the mobile phase; in acidic conditions, instead, the best enantioseparation of the aminoalcohols was achieved on cellulose tris (3, 5-dimethylphenilcarbamate). A long equilibration time of the CSP when switching from an undoped mobile phase to a doped one is required to obtain reproducible results.
使用两种多糖衍生的手性固定相(CSP)和各种含有酸性(TFA)或碱性(DEA)添加剂的正己烷/异丙醇流动相,在正相模式下实现了N-苄基-α-甲基苄胺、苯丙氨醇、色醇、2-(二苯基羟甲基)吡咯烷和异丙肾上腺素的HPLC对映体分离。这些化合物无需任何衍生化即可分离,分离因子范围在2.09至1.09之间,分辨率因子分别为3.4和0.4。在流动相中添加TFA的直链淀粉三(3,5-二甲基苯基氨基甲酸酯)CSP上实现了胺对映体的最佳分离;相反,在酸性条件下,在纤维素三(3,5-二甲基苯基氨基甲酸酯)上实现了氨基醇的最佳对映体分离。从未掺杂的流动相切换到掺杂的流动相时,CSP需要较长的平衡时间才能获得可重复的结果。