1,4-二氢吡啶类钙拮抗剂在超临界色谱中的对映体分离

发布时间：2018-03-02 11:08

本文关键词： -二氢吡啶类钙拮抗剂尼索地平西尼地平普拉地平阿折地平盐酸马尼地平手性拆分对映体分离超分子作用超临界流体色谱改性剂纤维素-三-(-甲基苯甲酸酯) 手性固定相　出处：《药物分析杂志》2017年08期 　论文类型：期刊论文

【摘要】：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。
[Abstract]:Objective: to establish a supercritical fluid chromatography (SCF) method for the chiral separation of 1 chloride-4-dihydropyridine calcium antagonist, and to explore its chiral recognition mechanism based on the mechanism of supramolecular interaction. Methods: supercritical fluid chromatography was used. Using supercritical carbon dioxide as mobile phase, the mobile phase was used as mobile phase with a flow rate of 2 mL 路min ~ (-1) and detection wavelength of 237 nm. The enantiomeric separation of five kinds of 1zodipine (nisoldipine, cilnidipine, Pradipine, azodipine, Manidipine hydrochloride) on Sino-Chiral OJ chiral column was studied. The effects of different modifiers (methanol, ethanol, isopropanol, ratio and system back pressure 1317 MPA) on the separation were also investigated. Baseline separation was achieved within 30 min (degree of separation 1.5, nisoldipine, cilnidipine, Pradipine, azodipine, azodipine). The optimized modifiers for Manidipine hydrochloride are carbon dioxide isopropanol 92: 8, carbon dioxide methanol 84: 16, carbon dioxide ethanol 74: 26, carbon dioxide ethanol 74: 26, carbon dioxide ethanol 74: 26, carbon dioxide ethanol 74: 26. Research shows that with the increase of the ratio of modifiers, The capacity factor gradually decreased, the elution ability of methanol and ethanol for 1hp 4-DHPs was always greater than that of isopropanol, and the higher the back pressure of the system, the faster the peak rate. Conclusion the separation of the enantiomers of 1: 1 4-DHPs by supercritical fluid chromatography is efficient and rapid. The recognition mechanism has certain guiding significance for the resolution of similar compounds.
【作者单位】：浙江工业大学环境学院;
【基金】：浙江省自然科学基金(No.Y506264)
【分类号】：O652.6;R917

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