【摘要】 利用配合交换原理，采用手性流动相添加剂方法，在反相高效液相色谱（ＲＰ－ＨＰＬＣ）制备柱上，拆分了氧氟沙星的两种对映体。流动相组成为手性添加剂溶液（含６ｍｍｏｌ／ＬＬ－苯丙氨酸和３ｍｍｏｌ／ＬＣｕＳＯ４）－ＣＨ３ＯＨ（８４：１６），流速４．６ｍＬ／ｍｉｎ，紫外检测波长２９３ｎｍ。经提取纯化后，确证首先洗脱的是Ｓ－（＋）－氧氟沙星，后一个洗脱的是Ｒ－（＋）－氧氟沙星。经对映体选择性分析方法测定，制备获得的两种对映体的光学纯度均大于９９％。更多还原

【Abstract】 Ofloxacin, （±）-9-fluoro-3-methyl-10-（4-methyl-1-piperazinyl）-7-oxo-2 , 3-dihydro-7 H-pyrido（1,2, 3-de）-1, 4-benzoxazine-6-carboxylic acid , has an asymmetric center at the C3 position in oxazine ring. In this paper ,a preparative high performance liquid chromatographic （HPLC）method for resolution of the enantiomers of （±）-ofloxacin using ligand-exchange chromatography,with L-phenylalanine-Cu（Ⅱ）as a chiral additive in mobile phase is presented. The preparative chiral HPLC conditions were cohimn:Shim-pack PREP-ODS （25cm×20mm i. d.）;mobile phase:6mmol/L L-phenylalanine and 3mmol/L copper sulphate containing 14% methanol;flow rate:4. 6mL/min; detector:fluorescence λ_ex=330nm, λ_em=505nm) . The eluates containing ofioxacin enantiomer were collected separately. The methanol was removed from the mobile phase in a water bath at 45℃ under vacuum and the residue was saturated with ammonium acetate. The enantiomer was extracted with methylene chloride （4×50 mL）. The organic solvent was evaporated to a small volume at 45℃ under vacuum. Anhydrous sodium sulfate was added and the liquid was then filtered. The filtrate was evaporated to dryness at 45℃.The residue was further dried over phosphorus pentoxide in a vacuum desiccator. The optical purity of each enantiomer was more than 90%.更多还原