文献类型：期刊文献

英文题名：Keywords: ?-cyclodextrin Chromatography stationary phase Two-dimensional separation Bufadienolides Bidirectional

作者：Sheng, Qianying[1];Wang, Ling[1];Zhang, Leyuan[1];Wang, Xue[2];Qian, Shengxu[2];Lan, Minbo[1];Qing, Guangyan[2];Liang, Xinmiao[2]

机构：[1]East China Univ Sci & Technol, Sch Chem & Mol Engn, Shanghai Key Lab Funct Mat Chem, Shanghai 200237, Peoples R China;[2]Chinese Acad Sci, Dalian Inst Chem Phys, Key Lab Separat Sci Analyt Chem, 457 Zhongshan Rd, Dalian 116023, Peoples R China

年份：2022

卷号：1673

外文期刊名：JOURNAL OF CHROMATOGRAPHY A

收录：;WOS:【SCI-EXPANDED(收录号:WOS:000830047700003)】；

基金：Acknowledgements This work was supported by the National Natural Science Foun-dation of China (21775116 , 21804041 , 21922411 and 21934005) , DICP Innovation Funding (DICP-RC201801) and LiaoNing Revitaliza-tion Talents Program (XLYC1802109) .

语种：英文

外文关键词：?-cyclodextrin; Chromatography stationary phase; Two-dimensional separation; Bufadienolides; Bidirectional

摘要：Natural products are rather complex samples containing a large number of compounds ranging from polar to nonpolar, small molecules to macromolecules, as well as numerous homologs/analogs with quite similar structures, which create great opportunities and treasures for discovery of bioactive drugs. For the purpose of better understanding the complex natural products and controlling their qualities, powerful analytical techniques for adequately separating chemical constituents and tracking potentially bioactive components are quite essential. Here, a design concept of bidirectional fi-cyclodextrin ( fi-CD)-modified chromatographic stationary phase toward separation of bufadienolides extracted from toad is proposed. Bufadienolides could be divided into two classes: toad venom ligand (AAUBs) and toad toxin (AACBs) with remarkable differences in structures and polarity. The hydrophobic cavity of fi-CD can encapsulate the steroid part of AACBs while the hydroxyls exposed on the fi-CD surface have strong hydrophilic interactions with the arginine part of AACBs. Isothermal titration calorimetry and hydrogen nuclear magnetic resonance titration experiment further validate the rationality of this design. Furthermore, the fi-CDbased stationary phase can be used as a hydrophilic material to construct a HILIC x RPLC 2D separation mode for the separation of AACBs, also works as a reverse phase material to construct a RPLC x RPLC 2D separation mode for the separation of AAUBs with good orthogonality. This study will open an avenue and provide a novel insight for high-efficiency two-dimensional separation of natural products. (c) 2022 Elsevier B.V. All rights reserved.