Electron spin resonance studies under dynamic mobile phase conditions on chemically modified silica.

Electron spin resonance studies under dynamic mobile phase conditions on chemically modified silica.
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化学改性二氧化硅动态流动相条件下的电子自旋共振研究。

DOI:
10.1016/s0021-9673(00)90569-7
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发表时间:
1988
期刊:
Journal of chromatography
影响因子:
--
通讯作者:
Gorse,J
Gorse,J
中科院分区:
--
文献类型:
--
作者:
Miller,C;Dadoo,R;Kooser,RG;Gorse,J

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电子自旋共振(ESR)技术的自旋标记和探测被证明是强大的方法,用于研究键合二氧化硅在动态溶剂流动条件下的色谱分离。从这些研究中获得的微观信息包括键合相的溶剂化组合物在键合相中的各个位置,键合相的配置和溶剂流动效应。在自旋标记研究中,使用2-(2,2_二甲基恶唑烷-N-氧基)己基硅烷(DOXYL己基硅氧烷)作为标记。ESR光谱显示键合表面的运动自由度作为移动的相组成和洗脱时间的函数的变化,并证明链硬化与水的引入,如由其他研究推断。在自旋探针工作中,在流动条件下将2,2,6,6-四甲基-1-哌啶氧基(TEMPO)家族的各种氮氧化合物作为0.1 mM溶液引入各种水-甲醇移动的相中。用该混合物平衡C18样品柱。光谱的解释产生了关于表面上的溶剂化环境的信息,所述表面上的溶剂化环境由探针采样作为探针的移动的相和极性的函数。
The electron-spin resonance (ESR) techniques of spin labeling and probing are shown to be powerful methods for the study of bonded silicas used in chromatographic separations under dynamic solvent flow conditions. Microscopic information gained from these studies includes solvation composition of the bonded phase at various locales in the bonded phase, configuration of the bonded phase and solvent-flow effects. In the spin-label study,2-(2,2-dimethyloxazolidine-N-oxy)hexylsilane (DOXYL hexyl siloxane) was used as the label. ESR spectra show changes in the motional freedom of the bonded surface as a function of mobile phase composition and elution time and demonstrate chain stiffening with the introduction of water, as infered by other studies. In the spin-probe work, various nitroxide compounds of the 2,2,6,6-tetramethyl-l-piperidinyloxyl (TEMPO) family were introduced under flow conditions as a O.1 mMsolution in various water—methanol mobile phases. C18sample columns were equilibrated with this mixture. Interpretation of the spectra yielded information about the solvated environment on the surface that was sampled by the probes as a function of both the mobile phase and the polarity of the probe.
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