高效液相色谱手性流动相添加法拆分2-苯丙酸对映体  

High performance liquid chromatographic enantioseparation of 2-phenylpropionic acid using chiral mobile phase additive

作　　者：郑烨[1] 颜继忠[1] 童胜强[1] 李行诺[1] 楚楚[1] 

机构地区：[1]浙江工业大学药学院,杭州310032

出　　处：《药物分析杂志》2013年第5期827-830,共4页Chinese Journal of Pharmaceutical Analysis

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)资助

摘　　要：目的:采用C18反相色谱柱,以羟丙基-β-环糊精作为手性流动相添加剂,建立了2-苯丙酸对映体的高效液相色谱拆分方法。方法:考察了羟丙基-β-环糊精的浓度、流动相pH、流动相中甲醇的比例、流动相流速和柱温对手性分离的影响,同时探讨了高效液相色谱采用羟丙基-β-环糊精分离2-苯丙酸对映体的分离机制及包结常数的计算,确定了色谱条件为YMC-Pack ODS-A C18(5μm,150 mm×4.6 mm)色谱柱,流动相为0.5%乙酸(pH 4.0,三乙胺调节)含25 mmol.L-1羟丙基-β-环糊精-甲醇(85∶15,v/v),流速为0.8 mL.min-1,柱温为45℃,紫外检测波长为254 nm。结果:(R,S)-2-苯丙酸的保留时间分别为15.85 min和17.57 min,分离度为1.50。结论:本方法分离度好,简便易行,且比手性固定相经济。Objective：To establish a method for enantioseparation of 2 -phenylpropionic acid（2 -PPA）using high performance liquid chromatography with hydroxypropyl -β -cyelodextrin （HP -β -CD） as the chiral mobile phaseadditive and a C18 reversed -phase column as the stationary phase. Methods ：The influences of the concentration of HP -β - CD, pH value of aqueous phase, methanol content, flow rate and column temperature on the peak resolutionwere investigated ,and the mechanism of inclusion complex between HP-β- CD and 2 -phenylpropionic acid was studied by HPLC. The enantiomers separation was carried out on a YMC -Pack ODS -A C18 （5μm,150 mm×4.6 mm） column with chiral mobile phase consisted of 0. 5% triethylamine acetate buffer （pH 4. 0） containing 25 mmol·L^-1 HP -β - CD - methanol （85：15 ,v/v）. The detecting wavelength was 254 nm. The flow rate was set at 0. 8 mL·min^-1 and the column temperature was 45 ℃. Results：The retention time of R -2 -phenylpropionic acid and S -2 - phenylpropionie acid were 15.85 min and 17. 57 min, and the resolution of 1.50 was achieved. Conclusion：The estab-lished method is simple, economic and with a good resolution.

关 键 词：高效液相色谱手性流动相添加法 2-苯丙酸 对映体拆分 羟丙基-Β-环糊精 

分 类 号：R917[医药卫生—药物分析学]