目的：建立超临界流体色谱法手性分离1，4-二氢吡啶类钙拮抗剂（1，4-DHPs），并基于超分子作用机制对其手性识别机理进行初步探讨。方法：采用超临界流体色谱法，以超临界二氧化碳作为流动相，流动相流速2 mL·min-1，检测波长237 nm，研究5种1，4-DHPs（尼索地平、西尼地平、普拉地平、阿折地平、盐酸马尼地平）在Sino-Chiral OJ手性色谱柱上的对映体分离，并考察不同改性剂种类（甲醇、乙醇、异丙醇）、比例以及系统背压（13~17 MPa）对分离效果的影响。结果：5种1，4-DHPs在柱温为35℃，系统背压为15 MPa时，在30 min内均实现了基线分离（分离度 > 1.5），尼索地平、西尼地平、普拉地平、阿折地平、盐酸马尼地平优化改性剂依次为二氧化碳-异丙醇（92：8）、二氧化碳-甲醇（84：16）、二氧化碳-乙醇（74：26）、二氧化碳-乙醇（74：26）、二氧化碳-乙醇（74：26）。研究发现，随着改性剂比例的增大，容量因子逐渐减小；甲醇和乙醇对1，4-DHPs的洗脱能力始终大于异丙醇；系统背压越大，出峰速度越快。结论：1，4-DHPs对映体在超临界流体色谱上可得到高效、快速的分离，其识别机理对同类化合物的拆分具有一定指导意义。
Objective: To establish the methods for enantioseparation of five 1, 4-dihydropyridinescalcium antagonist(1,4-DHPs)by supercritical fluid chromatography(SFC)on chiral stationary phase,and to explore the seperationmechanism based on supermolecular chemistry.Methods: Five 1, 4-DHPs(nisoldipine, cilnidipine, pranidipine,azelnidipine,manidipine hydrochloride)were separated by supercritical fluid chromatography(SFC) with supercritical carbon dioxide on a Sino-Chiral OJ column atthe flow rate of 2 mL·min-1 at the temperature of 35℃ and the UV detection was set on 237 nm. The effect of different type and percentage of modifiers(methanol, ethanol, isopropanol)and back pressure(13-17 MPa)on the separation was also investigated.Results: All the 1, 4-DHPs were obtained from the optimal separation(resolution >1.5)with the back pressure of 15 MPa and ratioof carbon dioxidide-isopropanol(92:8), carbon dioxidide-methanol(84:16), carbon dioxidide-ethanol (74:26),carbon dioxidide-ethanol(74:26), carbon dioxidide-ethanol(74:26),respectively. The study found the decrease of capacity factor was with the increase of modifiers' percentage, and the higher the back pressure of the system,the faster the peak of the 1, 4-DHPs eluted. The elution capacity of both methanol and ethanol was more effective than that of isopropanol.Conclusion: DHPs can be separated by SFC effectively and quickly,and the separation mechanism can be used as guidance for the same kind of compounds.
