Key Laboratory of Chemistry of Northwestern Plant Resources and Key Laboratory for Natural Medicine of Gansu Province, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China; University of Chinese Academy of Sciences, Beijing 100049, China.
Standardization Research Institute of Petroleum Industry, Research Institute of Petroleum Exploration & Development, Beijing 10083 China.
J Chromatogr A. 2019 Nov 8;1605:360357. doi: 10.1016/j.chroma.2019.07.011. Epub 2019 Jul 16.
A polyacrylamide (PAM)-coated silica packing as a novel stationary phase for hydrophilic interaction liquid chromatography (HILIC) was produced firstly by thermal immobilization. The coated layer was formed by a simple and facile physical method that dipping silica spheres into a PAM solution and then stirring the mixture until the solution was evaporated absolutely, leaving a certain amount of PAM on the silica particles. Although there are no chemical bonds involved, the bleeding measurement and the background noise are acceptable. Polyacrylamide coated silica (PAM-Sil, mean diameter: 5 μm) demonstrated a good hydrophilic property and excellent separation efficiency, which was observed especially for several high polar analytes such as saccharides. It is much higher than bare silica or amino columns under the same conditions. Moreover the obtained stationary phase demonstrated good stability under our operation conditions. The specific preparing method offers an easy and economical way to manipulate the thickness of PAM coating and can be extended as a universal way to produce various polymer coated stationary phases with dipping-heating/stirring-evaporating procedure.
首先通过热固定化制备了一种涂覆有聚丙烯酰胺（PAM）的硅胶填充剂，用作亲水相互作用液相色谱（HILIC）的新型固定相。涂覆层是通过一种简单易行的物理方法形成的，即将硅胶球浸入 PAM 溶液中，然后搅拌混合物，直到溶液完全蒸发，在硅胶颗粒上留下一定量的 PAM。尽管没有涉及化学键，但渗滤测量和背景噪声是可以接受的。涂覆有聚丙烯酰胺的硅胶（PAM-Sil，平均直径：5μm）表现出良好的亲水性和优异的分离效率，特别是对几种高极性分析物（如糖）具有良好的分离效果。在相同条件下，其分离效率远高于裸硅胶或氨基柱。此外，在我们的操作条件下，所得到的固定相表现出良好的稳定性。这种特定的制备方法提供了一种简单且经济的方法来控制 PAM 涂层的厚度，并且可以扩展为使用浸渍-加热/搅拌-蒸发程序制备各种聚合物涂覆固定相的通用方法。
