【摘要】 讨论了影响复杂游离地卟啉混合物高效液相色谱(HPLC)分析效果的主要因素,指出二溶剂梯度洗脱体系和三溶剂梯度洗脱体系有着实际的差异,不能简单地等同看待;流动相的溶剂配比是控制分析效果的决定性因素,同时,只有溶剂体系与洗脱梯度的有效配合才能取得良好的分析效果。探索了一套游离地卟啉二溶剂梯度HPLC分析条件。采用在流动相中同时加入醋酸和吡啶的方法,当溶剂A配比为正已烷∶二氯甲烷∶丙酮∶吡啶=500∶200∶50∶1.5,溶剂B配比为正已烷∶醋酸=105∶1时,采用使流动相起始极性较低的梯度洗脱方式,对于较低柱效的色谱柱(硅胶柱)亦能获得良好的分析效果。通过典型样品的质谱(MS)和HPLC的对比分析,给该分析条件下HPLC峰群进行了初步定性,认为对大多数地卟啉样品能实现ETIO,DPEP和Di-DPEP三种类型卟啉的较有效的分离。图5表3参4更多还原

【Abstract】 The differences between ternary and binary solvent system used for high performance liquid chromatographic (HPLC) analysis of metal-free geoporphyrins have been investigated, and shown that the ternary solvent system can not be equally treated as a binary one. A set of analytical conditions of binary solvent system analysis of complex mixture of metal-free geoporphyrins are set up. By varying the amount of both acetic acid and pyridine to the mobile phase, efficient separation can be achieved on lower efficience normal phase column through utilizing a proper stepped programme. By making a comparision between MS to HPLC of some typical samples, the HPLC peak groups of ETIO, DPEP and Di-DPEP are tentatively assigned, when the volume ratio of solvent mixtures used are: (A) hexane-methylene chloride-acetone-pyridine (500: 200: 50: 1.5), (B) hexane-acetic acid (105: 1).更多还原