Lesellier E, West C, Tchapla A
LETIAM, Groupe de Chimie Analytique de Paris Sud (EA 3343), IUT d'Orsay, Plateau du Moulon, Orsay, France.
J Chromatogr A. 2006 Apr 7;1111(1):62-70. doi: 10.1016/j.chroma.2006.01.107. Epub 2006 Feb 9.
Amongst the numerous base-deactivated ODS phases obtained by increasing the bonding density or/and by efficient endcapping treatments, some particular stationary phases have been developed, to limit the additional interactions of basic compounds with residual silanols, to work at extreme pH or with rich water mobile phases. Horizontal polymeric phases, sterically protected ones, hybrid silicas, propylene bridge, are particularly used for this purpose. Octadecyl chains with embedded polar groups and hydrophilic endcapping are also used in this goal. The properties of these phases were studied with a simple test consisting in the injection of carotenoid pigments in Subcritical Fluid Chromatography. The molecules used and the nature of the mobile phase allow the determination of hydrophobicity, polar site accessibility and type or/and bonding density of the stationary phases. Whatever the type of the phases, the particular stationary phases do not show any remarkable property, in comparison to other base-deactivated C18-bonded phases. On the other hand, embedded and polar-endcapped phases display a specific behaviour in regard of hydrophilic interactions, which are highlighted by the absence of water in the subcritical fluid. Additional properties of these phases are described, such as steric recognition and retention performances. As expected, polar-embedded phases are less retentive than classical ODS ones, but are sometimes able to provide greater steric recognition. On the other hand, the polar-endcapped phases display greater hydrophobicity than polar-embedded ones. From a simple classification diagram based on chromatographic properties, differences can be noticed between the polar-embedded groups (amide, carbamate, ether, sulfonamide) and between embedded and endcapped phases. Surprising behaviours are also noticed for some on the tested phases.
通过提高键合密度或/和采用有效的封端处理获得的众多碱钝化ODS固定相中,已开发出一些特殊的固定相,以限制碱性化合物与残留硅醇的额外相互作用,从而在极端pH条件下或使用富含水的流动相时发挥作用。水平聚合物固定相、空间保护型固定相、杂化硅胶、丙烯桥固定相尤其用于此目的。带有嵌入极性基团和亲水封端的十八烷基链也用于此目的。通过在亚临界流体色谱中注入类胡萝卜素色素的简单测试研究了这些固定相的性质。所使用的分子和流动相的性质可用于确定固定相的疏水性、极性位点可及性以及类型或/和键合密度。无论固定相的类型如何,与其他碱钝化C18键合固定相相比,这些特殊的固定相均未表现出任何显著特性。另一方面,嵌入型和极性封端型固定相在亲水相互作用方面表现出特定行为,这在亚临界流体中无水的情况下得以凸显。还描述了这些固定相的其他性质,如空间识别和保留性能。正如预期的那样,极性嵌入型固定相比传统的ODS固定相保留性更低,但有时能够提供更好的空间识别。另一方面,极性封端型固定相比极性嵌入型固定相具有更大的疏水性。从基于色谱性质的简单分类图中,可以注意到极性嵌入基团(酰胺、氨基甲酸酯、醚、磺酰胺)之间以及嵌入型和封端型固定相之间的差异。在所测试的一些固定相中还观察到了令人惊讶的行为。