氟西汀衍生物对映体在纤维素手性固定相上的拆分

Enantiomeric Separation of Derivatized Fluoxetine on Chiralcel OD Column

用纤维素 三 (3,5 二甲苯基氨基甲酸酯 ) (ChiralcelOD)手性固定相拆分了两种氟西汀衍生物对映体。使用 15cm长色谱柱分离NBD 氟西汀衍生物的流动相为四氢呋喃 /正己烷 (2 5∶75 ) ,分离DBD 氟西汀衍生物的流动相为四氢呋喃 /正己烷 (2 0∶80 ) ;流速为 1.0mL/min ,荧光检测 ,柱温为室温。醇类改性剂作流动相甚至不能部分拆分氟西汀衍生物。实验考察了四氢呋喃含量和柱长对手性分离的影响 ,探讨了手性拆分氟西汀衍生物的机理。

The derivatized fluoxetine with 4-(N-chloroformylmethyl-N-methyl) amino-7-nitro-2,1,3-benzoxadiazole (NBD-COCl) or 4-(N-chloroformethyl-N-methyl) amino-7-N, N-Dimethylamino-sulfonyl-2, 1, 3-benzoxadiazqle (DBD-COCl) was enantiomerically separated on cellulosed-based chiral stationary phase (Chiralcel OD) in the normal mode. For NBD-FLX, The better mobile phases used were tetrahydrofuran/hexane (25:75) on 15 cm OD column and for DBD-FLX, tetrahydrofuran/hexane (20:80) at a flow rate of 1.0 mL/min. The fluorescence detection was used. When alcohol modifiers such as methanol, ethanol, isopropanol, 1 butanol or tert-butanol were employed, no separation was observed. Effects of tetrahydrofuran content and column length on the separation,were examined Also, the separation mechanism of two derivatives on OD column was discussed.