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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
【摘要】 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。
【Abstract】 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-benzoxadiazole(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.
【Key words】 Fluoxetine; chiralcel OD; chiral stationary phase; enantiomeric separation;
- 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2004年10期
- 【分类号】O657.7
- 【被引频次】3
- 【下载频次】152