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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >A crosslinked, low pH-stable, mixed-mode cation-exchange like stationary phase made using the thiol-yne click reaction
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A crosslinked, low pH-stable, mixed-mode cation-exchange like stationary phase made using the thiol-yne click reaction

机译：交联，低pH稳定，混合模式交换，如静止相位使用硫醇-yne点击反应

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摘要

Mixed-mode cation-exchange stationary phases are useful for the separation of mixtures containing hydrophobic, acidic, and basic molecules. To ensure that weak organic bases are protonated and carboxylic acids are neutral low pH mobile phases are required. Mixed-mode stationary phases that are stable at pH < 3 are needed. We synthesized a crosslinked structure along the surface of thiol functionalized silica gel particles using the thiol-yne click reaction. The alkyne, 1,7-octadiyne, was added to the 3-mercaptopropyl silica gel, then crosslinked using 1,6-hexanedithiol. Elemental analysis showed low octadiyne ligand surface coverage, but, stoichiometrically, three sulfurs were added to each octadiyne ligand during the crosslinking step, indicating that crosslinking occurred. The effect of the crosslinking on the stability was tested with a 50:50 (v/v) pH 0.50 5% TFA aqueous:acetonitrile mobile phase at 70 degrees C for six days, over 35,0 00 column volumes. The stationary phase showed good stability with the retention of triphenylene decreasing only 20% during that time. The Tanaka test showed that the phase has a methylene selectivity of 1.20 +/- 0.04, a high shape selectivity of 2.71 +/- 0.03, and a 3.98 +/- 0.05 cation-exchange factor at pH 2.70. The phase has a selectivity factor for nitrobenzene and benzene of 1.41 +/- 0.01, indicating the electron donating charge transfer characteristic of the phase. The mixed-mode characteristics of the phase were investigated using a mixture of the monoamine neurotransmitters norepinephrine, dopamine, and serotonin. Baseline resolution of the monoamines could be obtained using a simple 20 mM potassium phosphate (pH 2.70)/methanol mobile phase. Altering both the methanol content and the potassium ion concentration altered the retention of the monoamines indicating mixed-mode cation exchange characteristic of the crosslinked stationary phase. (C) 2020 Elsevier B.V. All rights reserved.
机译：混合模式阳离子交换固定阶段可用于分离含有疏水性，酸性和碱性分子的混合物。为了确保质子化弱的有机碱而羧酸是中性低pH移动相。需要在pH <3时稳定的混合模式固定相。我们使用硫醇-YNE点击反应合成沿硫醇官能化硅胶颗粒表面的交联结构。将炔烃，1,7-八二腺苷加入到3-巯基丙基硅胶中，然后使用1,6-己二醇交联。元素分析显示出低碳含量配体表面覆盖，但是，在交联步骤期间，将三种硫加入到每个八达酰杨配体中，表明发生交联。交联对稳定性的效果用50:50（v / v）pH 0.50 5％TFA水溶液：乙腈流动相以70℃，六天以上，超过35,0 00柱。固定相表明，在此期间，三苯基的保留下降仅为20％的稳定性稳定性。 Tanaka试验表明，该相的亚甲基选择性为1.20 +/- 0.04，高形状选择性为2.71 +/- 0.03，pH 2.70的3.98 +/- 0.05阳离子交换系数。该相具有硝基苯和苯为1.41 +/- 0.01的选择性因素，表明相位的电子给予电荷转移特性。使用单胺神经递质去甲肾上腺素，多巴胺和血清素的混合物研究相相的混合模式特征。单胺的基线分辨率可以使用简单的20mM磷酸钾（pH2.70）/甲醇流动相来获得。改变甲醇含量和钾离子浓度改变了表明交联固定相的混合模式阳离子交换特性的单胺的保留。 （c）2020 Elsevier B.v.保留所有权利。

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