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用于亲水相互作用液相色谱的低出血极性固定相的制备。

Preparation of a low bleeding polar stationary phase for hydrophilic interaction liquid chromatography.

机构信息

Shanghai key Laboratory of new drug design, School of Pharmacy, East-China University of Science and Technology, Shanghai 200237, China.

Shanghai key Laboratory of new drug design, School of Pharmacy, East-China University of Science and Technology, Shanghai 200237, China.

出版信息

Talanta. 2018 May 15;182:500-504. doi: 10.1016/j.talanta.2018.01.009. Epub 2018 Jan 4.

DOI:10.1016/j.talanta.2018.01.009
PMID:29501185
Abstract

A common drawback of silica-based polar stationary phase is obvious bleeding, probably resulting from silica dissolution in water attracted onto silica gel. Recently we have reported a polyvinyl alcohol (PVA) encapsulated silica gel stationary phase for hydrophilic interaction liquid chromatography (HILIC), which demonstrated good chromatographic performance. Although PVA coating outside could shield SiO inside from erosion by aqueous solution to a certain degree, obvious bleeding of such phase was still observed. To eliminate or reduce the bleeding level of the phase, fabricating multi-layers of PVA coating crosslinked with glutaraldehyde onto silica gel is performed (PVA-GA-Sil). ∼20-fold decrease of the bleeding for PVA-GA-Sil can be achieved relative to bare silica gel, which is much lower than (or comparable to) commercial HILIC phases. PVA-GA-Sil also showed chromatographic performance and demonstrated superiority to commercial columns operated at gradient mode.

摘要

基于硅胶的极性固定相的一个常见缺点是明显的峰展宽,这可能是由于硅胶在被水吸引到硅胶上时溶解所致。最近,我们报道了一种用于亲水相互作用液相色谱(HILIC)的聚乙烯醇(PVA)包覆硅胶固定相,该固定相表现出良好的色谱性能。尽管 PVA 涂层的外侧可以在一定程度上屏蔽 SiO 内部免受水溶液的侵蚀,但仍观察到该固定相明显的峰展宽。为了消除或降低该固定相的峰展宽程度,对硅胶进行戊二醛交联的 PVA 涂层多层涂覆(PVA-GA-Sil)。与裸硅胶相比,PVA-GA-Sil 的峰展宽可降低约 20 倍,远低于(或可比于)商业 HILIC 相。PVA-GA-Sil 还表现出色谱性能,并在梯度模式下优于商业柱。

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