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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 m L·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 a chiral separation of 1,4-dihydropyridine calcium antagonists (1, 4-DHPs) by supercritical fluid chromatography and to investigate its chiral recognition mechanism based on supramolecular mechanism. Methods: Supercritical fluid chromatography with supercritical carbon dioxide as mobile phase was used. The mobile phase flow rate was 2 m L · min -1 and the detection wavelength was 237 nm. Five kinds of 1,4-DHPs (nisoldipine, Nifedipine, plydeidipine, aztredimin, manidipine hydrochloride) were separated on Sino-Chiral OJ chiral column and investigated the effect of different modifiers (methanol, ethanol and isopropanol) And system back pressure (13 ~ 17 MPa) on the separation effect. Results: Baseline separation (resolution> 1.5), nisoldipine, cilnidipine, pula (P <0.05) were achieved in all of the five 1,4-DHPs at a column temperature of 35 ℃ and a system backpressure of 15 MPa The results showed that the optimum conditions for the optimization of Manitopin Hydrochloride modifiers were carbon dioxide - isopropanol (92: 8), carbon dioxide - methanol (84:16), carbon dioxide - ethanol : 26), carbon dioxide-ethanol (74:26). The results showed that with the increase of the modifier, the capacity factor decreased gradually. The elution capacity of 1,4-DHPs from methanol and ethanol was always higher than that of isopropanol. The larger the back pressure was, the faster the peak was. Conclusion: The 1,4-DHPs enantiomers can be efficiently and rapidly separated by supercritical fluid chromatography. The recognition mechanism of 1,4-DHPs is helpful for the resolution of similar compounds.