高效液相色谱手性流动相添加法分离氟比洛芬对映体及其分离机制  

Enantioseparation of Flurbiprofen by High Performance Liquid Chromatography Using Chiral Mobile Phase Additive and Separation Mechanism

作　　者：沈芒芒[1] 郑烨[1] 颜继忠[1] 童胜强[1] 

机构地区：[1]浙江工业大学药学院,浙江杭州310032

出　　处：《浙江化工》2013年第4期28-31,共4页Zhejiang Chemical Industry

基　　金：国家自然科学基金(21105090);浙江省自然科学基金(Y4100472);浙江省科技厅项目(2010C33144)

摘　　要：以羟丙基-β-环糊精(HP-β-CD)为手性流动相添加剂,研究了氟比洛芬对映体在反相高效液相色谱中的拆分。考察了羟丙基-β-环糊精的浓度、流动相pH值、有机调节剂、柱温对手性分离的影响,同时探讨了HP-β-CD对氟比洛芬对映体在反相高效液相中的分离机制且计算出相应的包结常数。确定了色谱条件:YMC-Pack ODS-A C18(150 mm×4.6 mm,5μm)色谱柱,流动相为0.5%乙酸(pH3.5,三乙胺调节)含25 mmol/L羟丙基-β-环糊精:甲醇(80:20,v/v),流速为1.0 mL/min,柱温为30℃,紫外检测波长为247 nm。通过容量因子(k')的倒数1/k'对[HP-β-CD]的良好的线性关系证明氟比洛芬与HP-β-CD形成包结比为1:1包结物,(+)-氟比洛芬的包结常数为1.83 L/mol,(-)-氟比洛芬的包结常数为1.67 L/mol。The enantiomeric resolution of flurbiprofen was established by using reversed-phase high performance liquid chromatography with hydroxypropyl-β-cyclodextrin （HP-β-CD） as the chiral mobile phase additive. The influences of the concentration of HP-β-CD, the pH value, organic modifiers and column temperature on the resolution were investigated, and the separation mechanism of HPLC enantioseparation flurbiprofen using HP-β-CD is studied. The enantiomers separation was carried out on YMC-Paek ODS-A C18 （150 mm×4.6 mm,5μm） chromatographic column, and 0.5% triethylamine acetate buffer （pH3.5） containing 25 mmol/L hydroxypropyl-β-cyclodextrin： methanol = 80：20 （v/v）, the flow rate of 1.0 mL/min, column temperature of 30 ℃, UV detection wavelength of 247 nm. Graph of 1/k＇ vs [HP-β-CD] gave good linear relationships, indicating that the stoichiometry ratio of flurbiprofen and HP-β-CD is 1：1.The binding constants of （＋）-flurbiprofen is 1.83 L/mol, the binding constants of （-）-flurbiprofen is 1.67 L/mol.

关 键 词：包结常数 氟比洛芬 羟丙基-Β-环糊精 

分 类 号：TQ460.1[化学工程—制药化工] O657.72[理学—分析化学]