加压毛细管电色谱手性配体交换法对游离亮氨酸异构体分离的研究  

Enantiomeric Separation of Free Leucine by Pressurized Capillary Electrochromatography with Chiral Ligand Exchange Method

作　　者：辛艳飞[1,2] 万丽丽[3] 马丽萍[1] 孙烨[1] 周向军[1] 王永祥[1] 

机构地区：[1]上海交通大学药学院,上海200240 [2]浙江省医学科学院,浙江杭州310013 [3]上海交通大学第六人民医院药剂科,上海200030

出　　处：《分析测试学报》2008年第10期1088-1090,共3页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(30472052,30701064)

摘　　要：以反相C18为固定相，通过对流动相中的手性选择体、流动相组成与pH值及操作电压等条件的考察，成功建立了毛细管电色谱（CEC）手性配体交换法分离游离亮氨酸异构体的方法。优化的色谱条件：C18反相毛细管柱；以2mmol／L天冬氨酰苯丙氨酸甲酯为手性选择体，Cu^2＋为配体离子，流动相为20mmol／L乙酸缓冲液（pH5．5），5％（体积分数）的甲醇为有机改性剂；流速为0．02mL／min；操作压力为6．9×10^6 Pa；检测波长为UV 280nm；工作电压＋5kV；室温。两异构体可在15min内基线分离，检出限为10μmol／L（S／N=3），并在0．05～1．5mmol／L范围内呈良好的线性关系，日让、日内精密度均小于3．5％。A method for the separation of D-and L-leucine enantiomers by pressurized capillary electrochromatography with a chiral ligand exchange system using a chiral mobile phase additive and a[eversed-phase Cls column was established. An acetic buffer （20 mmol/L, pH 5.5 ）containing 2 mmol/L of aspartame, sufficiently complexed copper Ⅱ ions and methanol, was used as the mobile phase. The operation pressure and voltage were 6.9×10^6 Pa and ＋ 5 kV, respectively. The eluent was monitored with a UV detector at 280 nm. The separation was completed in 15 min. The standard curves of D/L-Leu ranged linearly from 0. 05 to 1.5 mmol/L （ r 〉 0. 99 ）. The within-day and between-day precisions of the quality control samples were less than 3.5% for both L-Leu and D-Leu.

关 键 词：亮氨酸 手性拆分 手性配体交换法 加压毛细管电色谱 

分 类 号：O657.8[理学—分析化学] Q517[理学—化学]