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D-2-烯丙基甘氨酸嵌入的咪唑桥联多面体低聚倍半硅氧烷杂化整体柱用于高效分离小分子和大分子。

D-2-allylglycine embedded imidazolium-bridged polyhedral oligomeric silsesquioxane hybrid monolithic column for efficient separation of both small molecules and macromolecules.

机构信息

Key Laboratory of Analytical Science and Technology of Hebei Province, College of Pharmaceutical Sciences, Hebei University, Baoding 071002, China.

Hebei Normal University Environmental Technology Co. Ltd., Shijiazhuang 050024, China.

出版信息

J Chromatogr A. 2020 Jan 4;1609:460491. doi: 10.1016/j.chroma.2019.460491. Epub 2019 Aug 27.

Abstract

The development of multifarious stationary phases is still a growing demand so as to solve the tasks of ever evolving actual applications. Herein, with D-2-allylglycine hydrochloride (AG·HCl) as the hydrophilic monomer, diene ionic liquid 1-allyl-3-vinylimidazolium bromide (AVI·Br) and polyhedral oligomeric silsesquioxane methacryl substituted (POSS-MA) as the dual crosslinkers, the highly cross-linked imidazolium-bridged POSS-AVI-AG hybrid monolithic column was fabricated via the "one-pot" free radical copolymerization. The AG·HCl embedded POSS-AVI-AG column displays typical reversed-phase liquid chromatography/hydrophilic interaction liquid chromatography mixed-mode retention mechanisms. Both hydrophobic phenols, alkylbenzenes, aromatic amines and hydrophilic nucleosides/nucleic acid bases, amides and thioureas were successfully separated with high column efficiencies (up to 571,000 plates/m for amides), outperforming our previously reported AVI·Br modified POSS-AVI column. Moreover, the column was also explored for the separation of cytochrome c tryptic digests and egg white protein extraction. All these results demonstrate that the POSS-AVI-AG column has a good potential in separation of both small molecules and complex biological samples with multiple mechanisms.

摘要

多种固定相的发展仍然是一个不断增长的需求,以解决不断发展的实际应用的任务。在此,以 D-2-烯丙基甘氨酸盐酸盐(AG·HCl)为亲水单体,二烯离子液体 1-烯丙基-3-乙烯基咪唑溴(AVI·Br)和多面体低聚倍半硅氧烷甲基取代(POSS-MA)为双重交联剂,通过“一锅法”自由基共聚制备了高度交联的咪唑桥联 POSS-AVI-AG 整体柱。AG·HCl 嵌入的 POSS-AVI-AG 柱显示出典型的反相液相色谱/亲水相互作用液相色谱混合模式保留机制。疏水性酚类、烷基苯、芳香胺和亲水性核苷/核酸碱基、酰胺和硫脲都可以用高柱效(最高可达 571000 板/m 用于酰胺)进行分离,优于我们之前报道的 AVI·Br 改性 POSS-AVI 柱。此外,该柱还用于细胞色素 c 酶解产物和蛋清蛋白提取的分离。所有这些结果表明,POSS-AVI-AG 柱在小分子和具有多种机制的复杂生物样品的分离方面具有良好的应用潜力。

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