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新型极性嵌入硅胶固定相的合成与表征及其在反相高效液相色谱中的应用。

Synthesis and characterization of novel polar-embedded silica stationary phases for use in reversed-phase high-performance liquid chromatography.

机构信息

Department of Chemistry, School of Pharmacy, Fourth Military Medical University, Xi'an 710032, China.

出版信息

J Chromatogr A. 2013 Jan 4;1271(1):153-62. doi: 10.1016/j.chroma.2012.11.045. Epub 2012 Nov 26.

Abstract

We have developed a series of new C(10) dipeptide stationary phases via a simple and effective synthetic method. The preparation of the new phases involves the synthesis of silanes and the surface modification of silica. Chromatographic evaluations of these columns were performed using the Engelhardt, Tanaka, and Neue test mixtures. The applicability of these new stationary phases was also evaluated using a series of diagnostic probes including acids, bases or neutral compounds and several generic applications. These new C(10) dipeptide stationary phases showed excellent hydrolytic stability over a wide pH range. Like other existing amide-embedded columns, these new stationary phases exhibit higher retention for polar and hydrophilic compounds and different selectivity as compared to conventional C(18) columns. These new phases are compatible with 100% aqueous mobile phases, and also provide 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系列新型 C(10)二肽固定相。这些新相的制备涉及硅烷的合成和硅胶的表面改性。使用 Engelhardt、Tanaka 和 Neue 测试混合物对这些柱进行了色谱评估。还使用包括酸、碱或中性化合物以及几种通用应用在内的一系列诊断探针评估了这些新固定相的适用性。这些新型 C(10)二肽固定相在很宽的 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,这些新型固定相对极性和亲水化合物具有更高的保留,并且与传统的 C(18)柱相比具有不同的选择性。这些新相与 100%水性流动相兼容,还可为酸性和碱性化合物提供高柱效和良好的峰形。

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