洛索洛芬钠的高效液相色谱手性拆分  

Chiral Separation of Loxoprofen Sodium by High Performance Liquid Chromatography

作　　者：丁文静[1] 郑文华[1] 许旭[1] 王德才[1] 吕龙[1] 梁宏晞[2] 郁韵秋[2] 阮锦满 

机构地区：[1]中国科学院上海有机化学研究所 [2]复旦大学药学院,上海200032 [3]南京宇道科技开发公司药物研究所,南京210018

出　　处：《分析化学》2004年第7期908-911,共4页Chinese Journal of Analytical Chemistry

基　　金：上海市自然科学基金资助项目 (No .0 1ZA14 0 77)

摘　　要：使用三 (对甲苯甲酸 )纤维素酯手性固定相 (ChiralcelOJ R手性柱 ) ,建立了洛索洛芬钠 4个手性异构体的高效液相色谱拆分方法。以甲醇与 pH 3.0的 0 .1mol/L醋酸 三乙胺或 0 .5mol/LHClO4 NaClO4按80∶2 0组成流动相 ,4个异构体中相邻峰的分离度均达到 1.7以上。确认了 4个组分的结构按出峰次序依次为 :(1′R ,2R)、(1′S ,2R)、(1′R ,2S)和 (1′S ,2S)。对流动相中不同的pH、缓冲溶液浓度和类型以及有机改性剂类型对分离结果的影响作了系统考察 ,其结果有助于更好地了解这类固定相的手性识别机理。A method for chiral separation of four loxoprofen sodium optical isomers was developed by high performance liquid chromatography on the chiral stationary phase of cellulose tris (4-methylbenzoate) (Chiralcel OJ-R). The effects of pH, concentration and type of the buffer, and organic modifier's kind in the mobile phase on the resolution and retention were investigated. The good resolution was obtained with the mobile phases of methanol/0.1 mol/L acetic acid-triethylamine (or 0.5 mol/L HClO4-NaClO4) at pH 3.0 = 80/20. The resolutions with over 1.7 for all continuous peaks were shown at. the mobile phase conditions. The peak sequence was identified as (1'R,2R), (1'S,2R), (1'R,2S.), (1'S,2S). The investigated results facilitate to understand the recognized mechanism of the cellulose-based chiral stationary phase.

关 键 词：洛索洛芬钠 高效液相色谱 手性拆分 非甾体抗炎药 三(对甲苯甲酸)纤维素酯手性固定相 

分 类 号：O657.3[理学—分析化学] TQ463[理学—化学]