【摘要】 用苯胺对3-叔丁基己二酸对映体进行柱前衍生后,在CHIRALCEL OD-H手性固定相上拆分,并通过二极管阵列紫外检测器和在线旋光检测器对其衍生物进行检测,首次建立了一种拆分3-叔丁基己二酸消旋体和测定3-叔丁基己二酸光学纯度的新方法。考察了流动相组成、柱温和流速对该对映体衍生物分离的影响。结果表明,3-叔丁基己二酸衍生物对映体在正己烷-异丙醇(体积比90∶10)为流动相,流速为1.0 mL.min-1,柱温为30℃时,分离效果最佳。在优化的实验条件下,分析在10 min内完成,分离因子和分离度均大于1.5。在质量浓度为2~160 mg/L范围内,(+)-3-叔丁基己二酸衍生物和(-)-3-叔丁基己二酸衍生物的回归方程分别为y1=2 116.4x1-3 541.3(r12=0.999 4)和y2=2 097.6x2-4 774.1(r22=0.999 1)。该方法操作简单、重复性好,可用于3-叔丁基己二酸对映体的质量控制。更多还原

【Abstract】 The 3-tert-butyladipic acid enantiomer was pre-column derivatized with aniline.The derivative was separated with CHIRALCEL OD-H chiral stationary phase,and detected by photo diode array detector and online optical detector.A high performance liquid chromatographic(HPLC) method for the separation of the racemate and the determination of the enantiomeric purity of 3-tert-butyladipic was established for the first time.The effects of chromatographic conditions,such as mobile phase,temperature and flow rate on chiral recognition,were investigated.A good separation was obtained at 30 ℃ by using hexane-isopropyl alcohol(90∶10,by volume) as mobile phase with a flow rate of 1.0 mL·min-1.Under the optimal conditions,the enantiomer was successfully separated in 10 min with separation factor and resolution more than 1.5.In the concentration range of 2-160 mg/L,the regression equations for the(+)-enantiomer derivative of 3-tert-butyladipic acid and the(-)-enantiomer derivative of 3-tert-butyladipic acid were y1=2 116.4x1-3 541.3(r21=0.999 4) and y2=2 097.6x2-4 774.1(r22=0.999 1),respectively.The presented study provided a simple and reproducible method for the enantiomeric quality control of 3-tert-butyladipic acid.更多还原