New oxo-bridged calix[2]arene[2]triazine stationary phase for high performance liquid chromatography.

New oxo-bridged calix[2]arene[2]triazine stationary phase for high performance liquid chromatography.
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用于高效液相色谱的新型氧桥杯[2]芳烃[2]三嗪固定相。

DOI:
10.1016/j.chroma.2011.12.031
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发表时间:
2012-02
期刊:
Journal of chromatography. A
影响因子:
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其他
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以3-氨丙基三乙氧基硅烷为偶联剂,制备了一种新型氧桥杯[2]芳烃[2]三嗪键合固定相(OCATS)。采用红外光谱、元素分析、热重分析等手段对新材料的结构进行了表征。以多环芳烃、单取代苯和双取代苯异构体为探针,在反相模式下考察了该固定相的色谱性能和保留机理,并与ODS进行了比较。新的OCATS固定相可以为不同的溶质提供各种相互作用,如疏水作用、氢键作用、ππ作用和包结作用。新材料中的芳香环、桥连氧原子、三嗪氮原子和烷基连接基团的协同作用通过多种保留机制提高了分离选择性。结合DFT-B3 LYP/STO-3G* 基团的量子化学计算结果,对分析物在OCATS柱上的保留行为进行了解释。OCATS色谱柱已成功应用于婴幼儿配方奶粉中三聚氰胺的分析。
A new oxo-bridged calix[2]arene[2]triazine bonded stationary phase (OCATS) for high performance liquid chromatography (HPLC) was prepared using 3-aminopropyltriethoxysilane as coupling reagent. The structure of new material was characterized by infrared spectroscopy, elemental analysis and thermogravimetric analysis. The chromatographic performance and retention mechanism of the new stationary phase were evaluated in reversed-phase mode compared with ODS using different solute probes including polycyclic aromatic hydrocarbons (PAHs), mono-substituted benzenes, disubstituted benzene isomers. The new OCATS stationary phase could provide various interactions for different solutes, such as hydrophobic, hydrogen bonding, ππ and inclusion interactions. The synergistic effects resulting from aromatic rings, bridging oxygen atoms and triazine nitrogen atoms and alkyl linkers in the new material improved the separation selectivity by multiple retention mechanisms. The retention behaviors of the analytes on OCATS column were explained with the assistance of quantum chemistry calculation results using DFT-B3LYP/STO-3G* base group. The OCATS column was successfully employed for the analysis of melamine in infant formula.
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