Development of a decaaza-cyclophane stationary phase for high-performance liquid chromatography
Development of a decaaza-cyclophane stationary phase for high-performance liquid chromatography
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高效液相色谱用十氮杂环芳固定相的开发
DOI：
10.1002/jssc.201400836
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发表时间：
2015-01-01
影响因子：
3.1
通讯作者：
Zhang, Shusheng
中科院分区：
文献类型：
--
作者：
Hu, Kai;Deng, Zhifen;Zhang, Shusheng
以3-氨基丙基三乙氧基硅烷为偶联剂，将杂原子桥联的环烷共价键合到硅胶上，制备了一种新型高效液相色谱固定相。通过红外光谱、元素分析和热重分析对新材料的结构进行了表征。线性溶剂化能关系法成功地用一组 25 种溶质评估了新相，并与十八烷基甲硅烷基和对叔丁基杯[4]芳烃键合固定相进行了比较。新相的保留特性与十八烷基甲硅烷基和传统的杯芳烃相相似，并且也具有鲜明的特点。此外，通过分别以反相模式和阴离子交换模式洗脱烷基苯和无机阴离子来说明该相的色谱行为。因此，新相的多重相互作用机制和混合模式分离很可能保证其在复杂样品分析中的应用前景。该色谱柱已成功用于牛奶中三嗪类化合物的分析，并被证明是测定三嗪类除草剂残留量的一种有竞争力的替代分析方法。
A new stationary phase for high-performance liquid chromatography was prepared by covalently bonding a heteroatom-bridged cyclophane onto silica gel using 3-aminopropyltriethoxysilane as the coupling reagent. The structure of the new material was characterized by infrared spectroscopy, elemental analysis, and thermogravimetric analysis. The linear solvation energy relationship method was successfully employed to evaluate the new phase with a set of 25 solutes, and compared with octadecylsilyl and p-tert-butyl-calix[4]arene bonded stationary phases. The retention characteristics of the new phase are similar to the octadecylsilyl and conventional calixarene phases, and it also has distinctive features. In addition, the chromatographic behavior of the phase was illustrated by eluting alkylbenzenes and inorganic anions in the reversed-phase mode and anion-exchange mode, respectively. Thus, multi-interaction mechanisms and mixed-mode separation of the new phase can very likely guarantee its promising application in the analysis of complex samples. The column has been successfully employed for the analysis of triazines in milk, and it is demonstrated to be a competitive alternative analytical method for the determination of triazine herbicide residues.