HPLC法测定(S)-2-氨基丁酰胺对映异构体  

A Validated RP-HPLC method using pre-column chiral derivatization for the detection of the enantiomer of (S)-2-Aminobutyramide hydrochloride

作　　者：苏江涛[1] 张登峰[1] 谢卫红[1] 糜志远[1] 张迎庆[1] 马卓[1] 

机构地区：[1]湖北工业大学食品与制药工程学院,武汉430068

出　　处：《分析试验室》2015年第10期1200-1203,共4页Chinese Journal of Analysis Laboratory

摘　　要：使用高效液相色谱-柱前衍生化法测定了（S）-2-氨基丁酰胺盐酸盐的对映异构体。采用梯度洗脱;流动相A为0.1 mol/L乙酸铵溶液,流动相B为乙腈溶液;流速1.5 m L/min;波长336 nm;柱温为40℃。（S）-2-氨基丁酰胺盐酸盐对映异构体的检出限和定量限分别为0.0085μg/m L和0.0319μg/m L。对映异构体的浓度在0.03~3.0μg/m L范围内线性关系良好（r2=0.9992）,回收率在91.8%~104.6%之间。方法能够有效控制左乙拉西坦重要中间体（S）-2-氨基丁酰胺的光学纯度。An RP-HPLC method was established for the determination of the（ R）-isomer of（ S）-2-aminobutyramide hydrochloride using pre-column chiral derivatization. 0. 1 mol / L ammonium acetate and acetonitrile were used as mobile phase A and B for the gradient elution. Flow rate was kept at 1. 5 m L / min,column temperature was set at 40 ℃ and UV detection wavelength was 336 nm. The LOD and LOQ were respectively 0. 0085 μg / m L and 0. 0319 μg / m L. The calibration curves of（ R）-isomer exhibited a good linearity in the range of 0. 03 μg / m L ~ 3. 0 μg / m L（ r2= 0. 9992）,and the recovery of（ R）-isomer was between 91. 8 %~ 104. 6 %. The method was validated and found to be precise,accurate and robust. The method can be used for the quality control of（ S）-2-aminobutyramide hydrochloride, the key intermediate for preparation of levetiracetam.

关 键 词：柱前衍生化 对映异构体 高效液相色谱 

分 类 号：TQ225.26[化学工程—有机化工]