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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Synthesis and chromatographic evaluation of a new stationary phase based on mild thiol-Michael addition reaction
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Synthesis and chromatographic evaluation of a new stationary phase based on mild thiol-Michael addition reaction

机译：基于轻度硫醇 - 迈克尔加成反应的新型固定相的合成与色谱评价

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摘要

Click chemistry has attracted increasing attention for the synthesis of novel stationary phases. Considering the advantage of click chemistry, a strategy based on thiol-Michael addition was developed for the preparation of a new stationary phase herein, and a phenyl vinyl sulfone stationary phase (M-PVS) was prepared. The resulting M-PVS bonded silica was characterized by elemental analysis, solid-state C-13 cross-polarization/magic-angle spinning NMR and infrared spectroscopy, confirming the successful immobilization of phenyl vinyl sulfone on the silica support. The retention properties of M-PVS were investigated and exhibited unambiguous reversed phase retention characteristics. Moreover, shape selectivity and silanol activity were studied to reveal the diverse interactions of M-PVS, including hydrophobic, pp, hydrogen bonding, and ion-exchange interactions. In addition, de-wetting tolerance and hydrophilic properties were evaluated and a pronounced "U" retention curves were obtained, indicating enhanced retention for polar analytes and transitions of different interaction modes. Selectivity differences between M-PVS column, phenyl column and conventional C-18 column were examined using series natural standards. The diverse interactions of M-PVS demonstrated its improved selectivity for the compounds with similar hydrophobic skeleton but different polar substituents. (C) 2019 Elsevier B.V. All rights reserved.Y
机译：点击化学引起了对新型固定阶段的合成的越来越关注。考虑到点击化学的优势，开发了一种基于硫醇-michael添加的策略，用于制备本文的新型固定相，制备苯基乙烯基砜固定相（M-PVS）。得到的M-PVS键合二氧化硅的特征在于元素分析，固态C-13交叉偏振/魔角纺丝NMR和红外光谱，证实苯基乙烯基砜的成功固定在二氧化硅载体上。研究了M-PVS的保留性能并表现出明确的反相保留特性。此外，研究了形状选择性和硅烷醇活性，以揭示M-PVS的不同相互作用，包括疏水性，PP，氢键和离子交换相互作用。此外，评价脱湿耐受性和亲水性，并获得明显的“U”保持曲线，表明对极性分析物的增强保留和不同相互作用模式的转变。使用系列自然标准检查M-PVS柱，苯基柱和常规C-18柱之间的选择性差异。 M-PVS的不同相互作用证明了其具有相似疏水性骨架但不同极性取代基的化合物的选择性。 （c）2019 Elsevier B.v.保留所有权利.Y

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