【摘要】 研究了11种碱性化合物在姜黄素键合硅胶固定相(CCSP)上的色谱行为,以ODS为参比,考察了流动相中甲醇含量、pH值对CCSP分离碱性物质的影响及CCSP的亲硅醇基活性,探讨了碱性物质在新固定相上的保留机理。结果表明,用不加缓冲盐的甲醇(含量分别为55%、40%、30%水)-二元流动相,未经封尾处理的姜黄素键合固定相能实现三组碱性化合物的基线分离。在相同色谱条件下,与ODS柱相比,CCSP对碱性物质具有较高的选择性,且N,N-二甲基苯胺和β-萘胺、N-甲苯胺和间硝基苯甲醛的洗脱顺序与ODS不一致,说明二者的保留机理有差异。新固定相对碱性化合物的分离除与疏水作用有关外,还与nπ-和π-π作用、偶极-偶极作用、氢键作用和电荷转移等作用有关。新固定相对碱性化合物分离具有两大优势:一是由于其较弱的疏水性和多种作用位点,有利于碱性化合物的快速分离;二是偶联剂间隔臂的屏蔽作用和配体的立体保护效应使硅醇基效应得到有效抑制,使得用单纯的甲醇-水流动相就能得到比在ODS上更对称的峰形,且碱性化合物的容量因子k′均随甲醇含量的增大而减小,并未出现"U"状。更多还原

【Abstract】 High-performance liquid chromatographic behavior of eleven basic compounds on a new curcumin bonded silica gel stationary phase(CCSP) was studied.The effects of mobile phase variables,such as methanol content and pH,on their chromatographic behavior,as well as the silanophilic activity of the CCSP were investigated.The retention behavior of the basic compounds was compared with that on ODS.The retention mechanisms of these solutes on the CCSP were also discussed.The results indicate that baseline separation of three series of basic compounds on the CCSP(no end-capped) can be achieved with methanol(55%,40%,30%,respectively)-water as a binary mobile phase without addition of a buffer solution.Compared with ODS,the CCSP exhibited better separation selectivity.Moreover,the elution orders of N,N-dimethylaniline and β-naphthylamine,N-methylaniline and m-nitrobenzaldehyde were very different under the same chromatographic conditions,which indicated that the two stationary phases under went different retention mechanisms in the chromatographic processes.According to the chromatographic data,the separation of the above compounds on the CCSP was based on hydrophobic interaction,n-π and π-π interactions,dipole-dipole interaction,hydrogen-bonding interaction,and charge transfer interaction.The CCSP has the advantages of fast and effective separation for basic compounds with more symmetrical peak shape using simple methanol-water mobile phase,and the capacity factor(k′) of these solutes decreases with the increase of methanol content on CCSP without occurrence of the "U" shape.更多还原