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合成了六个新型的1-取代苯基-4-[3-(吲哚-4-氧基)-2-羟丙基]-哌嗪消旋体化合物1–6,并利用键合型多糖手性固定相超临界流体色谱完成了对其的手性拆分研究。实验表明,基于固定相Chiralpak ⅠA的拆分优于其它两种键合型固定相(Chiralpak ⅠB、Chiralpak ⅠC),改性剂异丙醇的效果优于乙醇、甲醇、四氢呋喃、乙腈、二氯甲烷。本文还研究了有机改性剂、背压与柱温对六个化合物对映体拆分的影响。结果表明,改性剂组成最大程度地影响了分离时间,柱温的改变对分离时间的影响较小但最大程度地影响了对映体选择性的变化。最优的拆分条件为:固定相为Chiralpak ⅠA柱,柱温为35℃,背压为120bar,流动相为35%异丙醇(含0.1%二乙胺),流速为3.0mL/min,紫外检测波长为283nm。该六个消旋体化合物在10分钟内得到了良好的拆分。超临界流体色谱法是拆分该类化合物对映体的有效方法。
Six novel 1-substituted phenyl-4- [3- (indol-4-oxy) -2-hydroxypropyl] -piperazine racemate compounds 1-6 were synthesized, Chiral stationary phase supercritical fluid chromatography to complete its chiral resolution. Experiments show that the separation based on Chiralpak Ⅰ A is better than Chiralpak Ⅰ B and Chiralpak Ⅰ C. The isopropanol is better than ethanol, methanol, tetrahydrofuran, acetonitrile, methylene chloride . The effect of organic modifier, backpressure and column temperature on enantiomeric separation of six compounds was also studied. The results showed that the composition of modifier affected the separation time to a great extent. The change of column temperature had little effect on the separation time, but it affected the change of enantioselectivity to a great extent. The optimal conditions were as follows: the stationary phase was Chiralpak Ⅰ A column, the column temperature was 35 ℃, the back pressure was 120 bar, the mobile phase was 35% isopropanol with 0.1% diethylamine, the flow rate was 3.0 mL / min, UV detection wavelength of 283nm. The six racemic compounds are well resolved in 10 minutes. Supercritical fluid chromatography is an effective method for the resolution of enantiomers of these compounds.