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一种水解稳定的酰胺嵌入固定相的制备与评价

Preparation and evaluation of a hydrolytically stable amide-embedded stationary phase.

作者信息

Liu Xiaodong, Bordunov Andrei V, Pohl Christopher A

机构信息

Dionex Corporation, Sunnyvale, CA 94088, USA.

出版信息

J Chromatogr A. 2006 Jun 30;1119(1-2):128-34. doi: 10.1016/j.chroma.2005.11.086. Epub 2006 Feb 3.

Abstract

We have developed a new hydrolytically stable amide-embedded stationary phase via a simple and effective synthetic method. The preparation of the new phase involves the synthesis of multifunctional silane ligands and the surface modification of porous silica particles via multiple attachments of these ligands to the silica surface. A hydrolytically stable coating was produced as a result of multiple covalent linkages formed between silane ligands and the silica surface, and cross-linking between adjacent ligands. The resulting amide-embedded stationary phase showed excellent hydrolytic stability over a wide pH range. Like other existing amide-embedded columns, this new stationary phase exhibits higher retention for polar compounds and different selectivity as compared to conventional C18 columns. The new phase is compatible with 100% aqueous mobile phases, and also provides high column efficiency and good peak shapes for both acidic and basic compounds.

摘要

我们通过一种简单有效的合成方法开发了一种新型的水解稳定型酰胺嵌入固定相。新固定相的制备涉及多功能硅烷配体的合成以及通过这些配体与二氧化硅表面的多次连接对多孔二氧化硅颗粒进行表面改性。由于硅烷配体与二氧化硅表面之间形成了多个共价键以及相邻配体之间的交联,从而产生了一种水解稳定的涂层。所得的酰胺嵌入固定相在很宽的pH范围内表现出优异的水解稳定性。与其他现有的酰胺嵌入柱一样,这种新型固定相对极性化合物具有更高的保留能力,并且与传统的C18柱相比具有不同的选择性。新固定相与100%水相流动相兼容,并且对酸性和碱性化合物都具有高柱效和良好的峰形。

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