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L-cysteine and 5-Norbornene-2-carboxylic acid Decorated Mesoporous Silica Spheres as Liquid Chromatographic Material
Microporous and Mesoporous Materials ( IF 4.8 ) Pub Date : 2020-02-19 , DOI: 10.1016/j.micromeso.2020.110102
Fangbin Fan , Xiaobin Nie , Chao Fan , Xiaojing Liang , Xiaofeng Lu , Yong Guo

In this paper, L (+)-Cysteine (L-Cys) and 5-norbornene-2-carboxylic acid (5-N-2-CA) were modified on the silica spheres by cross-linking polymerization and thiol-ene click reaction. The Cys-Si-NCA was characterized by scanning electron microscopy, nitrogen sorption porosimetry, thermo gravimetric analysis and other characterization methods. The results indicated that the colume had a regular spherical shape with porous surfaces and particle sizes mainly ranging from 4.5 to 5.5 μm. The surface area of the Cys-Si-NCA microspheres was 328.68 m2 g-1, and their respective average pore size was 9.27 nm. Furthermore, the colume exhibited excellent stabilities and reproducibility. Experimental results demonstrate that this new stationary phase can facilitate the separation of sulfonamides, nucleosides and nucleobases compounds in hydrophilic chromatographic (HILIC) conditions. In addition to being able to attenuate the peak tailing of separation, it can also be used for quantitative analysis of creatinine in urine. We also give the temperature and pH ranges of separation on Cys-Si-NCA column. The successful synthesis of the Cys-Si-NCA stationary phase provides foundation for the application of this kind of materials in liquid chromatography (LC).



中文翻译:

L-半胱氨酸和5-降冰片烯-2-羧酸修饰的中孔二氧化硅球体作为液相色谱材料

本文通过交联聚合和硫醇-烯点击反应,在二氧化硅球上修饰了L(+)-半胱氨酸(L-Cys)和5-降冰片烯-2-羧酸(5-N-2-CA)。 。通过扫描电子显微镜,氮吸附孔隙率法,热重分析和其他表征方法对Cys-Si-NCA进行了表征。结果表明,该胶粒具有规则的球形形状,具有多孔表面,并且粒径主要在4.5至5.5μm的范围内。Cys-Si-NCA微球的表面积为328.68 m 2 g -1,并且它们各自的平均孔径为9.27nm。此外,该软胶表现出优异的稳定性和可再现性。实验结果表明,这种新的固定相可以在亲水色谱(HILIC)条件下促进磺酰胺,核苷和核碱基化合物的分离。除了能够减弱分离的峰拖尾,它还可以用于尿中肌酐的定量分析。我们还给出了在Cys-Si-NCA色谱柱上分离的温度和pH范围。Cys-Si-NCA固定相的成功合成为此类材料在液相色谱(LC)中的应用奠定了基础。

更新日期:2020-02-20
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