柱前衍生化-手性固定相法拆分2-甲基哌嗪对映体  

Enantioseparation of 2-methyalpiperazine by chiral stationary phase with pre-column derivatization

作　　者：李春香[1,2] 雷勇胜[2] 蒋庆峰[2] 

机构地区：[1]天津中医药大学研究生院,天津300193 [2]天津药物研究院,天津300193

出　　处：《化学试剂》2013年第1期68-70,共3页Chemical Reagents

摘　　要：以2,4-二硝基氟苯为衍生化试剂,建立柱前衍生化结合手性固定相高效液相色谱法拆分2-甲基哌嗪对映体的方法。采用Chiralpak IA(250 mm×4.6 mm,5μm)手性色谱柱,流动相为V(正己烷)∶V(无水乙醇)∶V(二乙胺)=50∶50∶0.1,检测波长261 nm,流速0.5 mL/min,柱温30℃。在此优化试验条件下,衍生后的对映体分离度达3以上,在0.15～1.5μg/mL浓度范围内线性关系良好,连续重复进样6次,相对标准偏差(RSD)在0.15%以下。该方法灵敏度高,重复性好,可用于2-甲基哌嗪异构体的质量控制。To establish a method for enantioseparation of 2- methyalpiperazine by chiral stationary phase with pre-column derivatization. 2,4-Difluoronitrobrnzene was took as the reagent for derivatization. Enatiomers of 2-methyalpiperazine were separated on a Chiralpak IA（250 ×4.6 mm,5 μm） column with a mobile phase consisting of hexane-ethanol-diethyl- amine（50：50： 0. 1） and wavelength was set at 261 nm. The flow rate was 0. 5 mL/min and the temperature of column was set at 30℃. It is concluded that at this optimized condition, the resolution of the derivated enantiomers was above 5, and the calibration curves of R-（ - ） 2-methyalpiperazine and S- （＋）-2-methyalpiperazine were linear in the concentration range of 0. 15 - i. 5 ixg/mL. After continuous injection for six times,the RSD was no more than 0. 15%. The method is sen- sitive and highly reproducible and is suitable for the quality control of 2-methyalpiperazine.

关 键 词：2-甲基哌嗪 对映体 柱前衍生化 手性固定相 正相高效液相色谱法(NP—HPLC) 

分 类 号：R9[医药卫生—药学]