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柱前衍生化-HPLC测定仲丁胺对映体的纯度
Determination of enantiomeric purity for 2-butylamine by HPLC combining with pre-column derivation
【摘要】 用3,5-二硝基苯甲酸对仲丁胺进行柱前衍生,将其衍生物在CHIRAL-CEL OD-H手性固定相上拆分,并通过二极管阵列紫外检测器对其衍生物进行检测,建立了一种拆分仲丁胺消旋体、测定仲丁胺光学纯度的新方法。以正己烷和乙醇或异丙醇为流动相,在CHIRALCEL OD-H手性固定相上对仲丁胺衍生物进行了拆分,并考察了流动相组成和柱温对该对映体衍生物分离的影响,获得较好的分析条件,分离因子大于1.2。非手性试剂柱前衍生化法测定仲丁胺光学纯度与旋光度方法比较,结果一致。方法可用于仲丁胺对映体的质量控制。
【Abstract】 2-Butylamine was derivatized with 3,5-dinitrobenzoic acid that was the reagent of pre-colume derivatization of high performance liquid chromatography.The derivative was separated by CHIRALCEL OD-H chiral stationary phase,and detected by a Photo-Diode-Array detector.A method for separating the racemate and determining the enantiomeric purity of 2-butylamine was established.Chromatographic model was employed for enantiomeric separation of 2-butylamine derivatives on the CHIRALCEL OD-H chiral colume in hexane/alcohol(ethanol or isopropyl alcohol) mobile phase.The effects of chromatographic conditions,such as mobile phase and temperature on chiral recognition,had been investigated.A better condition of analysis was obtained and the separation factor was more than 1.2.Furthermore,the results of enantiomeric purity determined by both polarimeter and HPLC were very consistent.The presented study provided a simple and reproducible method for the enantiomeric quality control of 2-Butylamine.
【Key words】 High performance liquid chromatography; Pre-colume derivatization; Chiral stationary phase; 2-Butylamine; Optical purity;
- 【文献出处】 分析试验室 ,Chinese Journal of Analysis Laboratory , 编辑部邮箱 ,2009年05期
- 【分类号】O657.72
- 【被引频次】8
- 【下载频次】238