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一锅法水热交联制备用于亲水作用色谱的聚乙烯基吡咯烷酮固定化硅胶固定相。

One-pot hydrothermal cross-linking preparation of poly(vinylpyrrolidone) immobilized silica stationary phase for hydrophilic interaction chromatography.

机构信息

CAS Key laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian, 116023, China; University of Chinese Academy of Sciences, Beijing 100049, China.

CAS Key laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian, 116023, China.

出版信息

J Chromatogr A. 2020 Dec 6;1633:461656. doi: 10.1016/j.chroma.2020.461656. Epub 2020 Oct 29.

Abstract

Hydrothermally cross-linked polyvinylpyrrolidone (PVP) immobilized SiO stationary phase (CPVP-Sil) was prepared via a green and facile one-pot method which was demonstrated for hydrophilic interaction liquid chromatography (HILIC) as well as reverse phase chromatography(RP). A water or organic solvent-insoluble permanent CPVP immobilizing on the silica particle surface can be formed simply by dipping silica particles into PVP solution and low temperature hydrothermal treatment. The cross-linked PVP network coating on SiO endow it ring lactam functional groups which exhibited excellent separation ability of polar compounds by a typical HILIC retention mechanism at higher organic solvent contents (>55% ACN) and additionally polyvinyl groups for separation of alkylbenzenes in RP mode(<25% ACN). A high column efficiency of about 7 × 10 plates per meter was obtained for the test catechol compound. Remarkably, the CPVP-Sil packing materials showed good stability in acid (at pH 3.5) or basic (at pH 9.5) conditions, with 5400-fold column volumes and 3500-fold column volumes respectively.

摘要

水热交联聚乙烯吡咯烷酮(PVP)固定相 SiO2(CPVP-Sil)通过绿色简便的一锅法制备,可用于亲水作用液相色谱(HILIC)和反相色谱(RP)。通过将硅胶粒子浸入 PVP 溶液并进行低温水热处理,简单地在硅胶粒子表面形成不溶于水或有机溶剂的永久 CPVP 固定化。交联的 PVP 网络涂覆在 SiO2 上,赋予其内酯官能团,通过典型的 HILIC 保留机制,在较高有机溶剂含量(>55%ACN)下,对极性化合物表现出优异的分离能力,此外,在 RP 模式下,通过聚亚甲基基团对烷基苯进行分离(<25%ACN)。用于测试儿茶酚化合物的色谱柱效率约为每米 7×10 个板。值得注意的是,CPVP-Sil 填充材料在酸性(pH 3.5)或碱性(pH 9.5)条件下具有良好的稳定性,分别具有 5400 倍和 3500 倍的柱体积。

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