【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2 mmol/L天冬氨酰苯丙氨酸甲酯为手性选择体,Cu2+为配体离子,流动相为20 mmol/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0.02 mL/min;操作压力为6.9×106Pa;检测波长为UV280 nm;工作电压+5 kV;室温。两异构体可在15 min内基线分离,检出限为10μmol/L(S/N=3),并在0.05~1.5 mmol/L范围内呈良好的线性关系,日间、日内精密度均小于3.5%。更多还原

【Abstract】 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 reversed-phase C18 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 6.9×106 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.更多还原