Stationary phases with chemically bonded fluorene ligands: A new approach for environmental analysis of pi-electron containing solutes
Stationary phases with chemically bonded fluorene ligands: A new approach for environmental analysis of pi-electron containing solutes
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DOI：
10.1016/s0021-9673(96)00682-6
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发表时间：
1997-01-03
影响因子：
4.1
通讯作者：
Klaus, A
中科院分区：
文献类型：
--
作者：
Brindle, R;Klaus, A
为了高效液相色谱（HPLC）分离含π电子的溶质，通过两步改性不同孔径的硅胶，制备了一种新的硅胶表面化学键合芴配体的固定相。通过固态核磁共振（NMR）光谱和HPLC对该新相进行了表征。色谱性能测定的三个测试混合物，两个含有多环芳烃（PAHs）和第三个含有硝基炸药的分离。的多环芳烃的洗脱顺序是相同的情况下，通常的反相，而硝基炸药的洗脱是反向的，因为强的π-π之间的相互作用的贫电子溶质和富电子的固定相。固体核磁共振弛豫时间的测量被用来研究键合的芴配体的动态行为。固态NMR调查的结果进行了讨论的各种HPLC分离的背景下。色谱和光谱性质都显示出对起始硅胶基质的孔径大小的依赖性。
For the separation of pi-electron-containing solutes by high-performance liquid chromatography (HPLC), a new stationary phase with a fluorene ligand chemically bonded to a silica gel surface was developed following a two-stage modification of silica gels with different pore sizes. This new phase was characterized by solid-state nuclear magnetic resonance (NMR) spectroscopy and HPLC. Chromatographic properties were determined by the separation of three test mixtures, two containing polycyclic aromatic hydrocarbons (PAHs) and the third containing nitro explosives. The elution order of the PAHs is the same as in case of usual reversed-phases, while the elution of the nitro explosives is inverted because of strong pi-pi interactions between the electron-poor solutes and the electron-rich stationary phase. Solid-state NMR relaxation time measurements were used to study the dynamic behaviour of the bonded fluorene ligands. The results of solid-state NMR investigations are discussed in the context of various HPLC separations. Both chromatographic and spectroscopic properties show a dependence on the pore size of the starting silica gel matrix.