柱前衍生化法结合HPLC测定2-哌啶乙醇对映体光学纯度

Determination of Enantiomeric Purity for 2-Piperidineethanol by HPLC Combining with Pre-Column Derivation

用3,5-二硝基苯甲酸对2-哌啶乙醇进行柱前衍生,将其衍生物在Chiralcel OD-H手性固定相上拆分,建立了一种拆分2-哌啶乙醇消旋体、测定2-哌啶乙醇光学纯度的新方法。以正己烷与乙醇或异丙醇为流动相,在Chiralcel OD-H手性固定相上对2-哌啶乙醇衍生物进行了拆分,并考察了流动相组成、柱温和流速对该对映体分离的影响,获得较优分析条件,分析时间在15分钟内,分离度大于1.7。结果表明,2-哌啶乙醇衍生物对映体在正己烷-乙醇(体积比85:15)为流动相、流速为1.0mL min-1、柱温为30℃时,分离效果最佳。本方法操作简单、重现性好,可用于2-哌啶乙醇对映体的质量控制。

The 2-piperidineethanol was derivatized with 3,5-dinitrobenzoic acid that was the reagent of precolume derivatization of high performance liquid chromatography, and the derivative was separated by Chiralcel OD-H chiral stationary phase. A method for separating the racemate and determining the enantiomerle purity of 2-piperidineethanol was established. Chromatographic model was employed for enantiomeric separation of 2-piperidineethanol derivatives on the Chiralcel OI）-H chiral colume in hexane/alcohol （ethanol or isopropyl alcohol） mobile phase. The effects of chromatography conditions, such as mobile phase, temperature and flow rate to chiral recognition, had been investigated. A better condition of analy- sis was obtained within a short run time of less 15 rain. The resolution were more than 1.7. The results indicated that a good separation was obtained at 30℃by usinghexane-ethanol （85： 15, V/V） as the mobile phase with a flow rate of 1.0 mL min-1. The presented study provided a simple and reproducible method for the enantiomeric quality control of 2-piperidineethanol.