咪唑嵌合半胱氨酸修饰固定相制备及色谱应用

Imidazolium-embedded cysteine-functionalized stationary phases: preparation and its chromatographic applications

利用“点击反应”合成了咪唑嵌合半胱氨酸硅胶固定相SIL-AVI-Cys,并通过热重、红外光谱以及元素分析对材料进行了表征.填充SIL-AVI-Cys色谱柱在分离胞核嘧啶、胞苷、肌苷、尿嘧啶和尿苷等5种亲水性化合物时表现为亲水作用模式,而在分离苯胺和苯酚类物质时则可表现出亲水/反相混合模式特征.通过考察流动相pH值、盐浓度对分析物保留的影响,进一步探讨了该固定相的分离机理.流动相pH值的改变可通过改变分析物的离子化影响其与固定相之间的作用力及其保留行为.流动相中盐浓度的增加,可减弱酸性分析物的保留,而对于碱性和中性分析物则无显著影响.此外,SIL-AVI-Cys色谱柱的分离性能采用酰胺及核酸碱基/核苷类物质进行了表征,并将其进一步应用于奶粉中三聚氰胺的表征和检测.

A novel imidazolium-embedded cysteine-functionalized stationary phase SIL-AVI-Cys was prepared by“click reaction”,which was further characterized by thermogravimetric analysis,FT-IR as well as elemental analysis.The stationary phase exhibits HILIC mode in the separation of five hydrophilic compounds,such as cytosine,cytidine,inosine,uracil and uridine,which also exhibits HILIC/RPLC mixed mode when separating anilines and phenolic substances.The separation mechanism of the stationary phase was further explored by investigating the effects of mobile phase pH and salt concentration on the retention of analytes.The change in the pH of the mobile phase can affect the interaction between analytes and the stationary phase by varying the dissociation of the analytes.The separation characteristics of the SIL-AVI-Cys column were also investigated by amides and nucleobases/nucleosides.The SIL-AVI-Cys column was further used for characterization and detection of melamine in baby milk powder.