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Synthesis and chromatographic characteristics of iminodisuccinic acid-functionalized silica stationary phase
Journal of Chromatography A ( IF 3.8 ) Pub Date : 2017-11-15 , DOI: 10.1016/j.chroma.2017.11.032
Bin Chen , Ning Zhang , Chen Li , Rong Li , An Fan

In this study, we developed a multifunctional chromatographic medium by using iminodisuccinic acid (IDS) as ligand, γ-glycidoxypropyltrimethoxysilane (γ-GLDP) as spacer arm and silica as matrix. The medium was characterized by fourier transform infrared spectrometry (FT-IR). Binding capacity of IDS on chromatographic medium was determined by potentiometric titration. The effect of mass ratios (w/w) between silica and IDS on the medium synthesis was discussed. The optimal ratio of matrix, spacer arm and ligand was 1.5 g: 2.0 mL: 4.6 g. Based on different chromatographic modes, protein mixtures of bovine serum albumin, ribonuclease and lysozyme were successfully separated with IDS-Silica column and IDS-Cu(II)-Silica column, respectively. To examine metal chelating behavior of IDS-Silica stationary phase, optimal geometries and related parameters of complexes formed by IDS with Fe3+, Cu2+, Ni2+, Zn2+, Co2+ and Ca2+ were achieved by quantum computing. The stabilities of the complexes were predicted according to the results of theoretical calculation. Sorption capacities of IDS-Silica stationary phase for metal ions were determined by using offline frontal chromatography (FC) combined with inductively coupled plasma atomic emission spectrometry (ICP-AES). A good agreement was found between simulating results and experimental observations. The order of chelating strength of IDS-Silica medium for metal ions was Fe3+ > Cu2+ > Ni2+ > Zn2+ > Co2+ > Ca2+. Compared with IDA-Silica, Asp-Silica and Glu-Silica stationary phases, IDS-Silica displayed a stronger chelating property for metal ion.



中文翻译:

亚氨基二琥珀酸官能化的硅胶固定相的合成及色谱特性

在这项研究中,我们以亚氨基二琥珀酸(IDS)为配体,以γ-环氧丙氧基丙基三甲氧基硅烷(γ-GLDP)为间隔臂,以二氧化硅为基质,开发了一种多功能色谱介质。该介质通过傅立叶变换红外光谱法(FT-IR)表征。通过电位滴定法确定IDS在色谱介质上的结合能力。讨论了二氧化硅和IDS之间的质量比(w / w)对介质合成的影响。基质,间隔臂和配体的最佳比例为1.5 g:2.0 mL:4.6 g。根据不同的色谱模式,分别用IDS-硅胶柱和IDS-Cu(II)-硅胶柱成功分离了牛血清白蛋白,核糖核酸酶和溶菌酶的蛋白质混合物。要检查IDS-二氧化硅固定相的金属螯合行为,通过量子计算获得了3+,Cu 2 +,Ni 2 +,Zn 2 +,Co 2+和Ca 2+。根据理论计算结果预测了配合物的稳定性。IDS-硅胶固定相对金属离子的吸附能力是通过使用离线额叶色谱(FC)结合电感耦合等离子体原子发射光谱法(ICP-AES)来确定的。在模拟结果和实验观察之间发现了很好的一致性。IDS-二氧化硅介质对金属离子的螯合强度顺序为Fe 3+  > Cu 2+  > Ni 2+  > Zn 2+  > Co 2+ > Ca 2+。与IDA-Silica,Asp-Silica和Glu-Silica固定相相比,IDS-Silica对金属离子具有更强的螯合性能。

更新日期:2017-11-15
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