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Calixarene Derivatives Analysis And Their Applications In Nonaqueous Capillary Electrophoresis

Posted on:2008-12-01Degree:MasterType:Thesis
Country:ChinaCandidate:P HanFull Text:PDF
GTID:2121360215461337Subject:Analytical Chemistry
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Nonaqueous capillary electrophoresis(NACE) was firstly introduced by Walbroehl and Jorgenson in 1984. The benefits of NACE have been described in a number of recent publications, such as the wide use of organic solvents, the lower current present, the high selectivity and easily coupling with MS detection, NACE has become an active area in analytical chemistry. As a typical representative of the third generation of supramolecules, calixarenes have been increasingly attracting attentions. The use of calixarenes in separation sciences is in the process of development. The calixarene analysis and its application in NACE have been carried out in three aspects as follows:1. Four groups of hydrophobic calixarenes were separated by nonaqueous capillary electrophoresis(NACE). The effect of nonaqueous solvent, pH~* and concentration of buffer on the resolution was investigated, and the optimal conditions were obtained. Using the optimal separation conditions, complete separations of these calixarenes were achieved, and a simple, fast, high sensitive and strong adaptive method for separation of hydrophobic calixarene was established,2. Three groups of calixarenes with different structures were analyzed by electrosprayion trap mass spectrometry (ESI-ITMS), and their MS cleavage pathways were investigated. The results show that calixarenes easily formed molecular ion ([M-H]~-) in negative detection mode. In MS~n collision induced detection, their characteristic were obtained. This method provides reliable qualitative and quantitative strategy of those calixarenes.3. Four calixarenes and one resorc[4]arene were investigated in the separations of twobinaphthaline derivatives by nanaqueous capillary electrophoresis(NACE). The results show that p-sulfocalix[6]arene was the most capable selector for all the BINOL and BNA. Electrophoretic parameters such as the detection wavelength, the organic solvent, the concentration of the chiral selector and the pH~* value were optimized. Incresing the concentration up to 10mmol/L of p-sulfocalix[6]arene led to high separation efficiency. Using Gaussview 03 software, the structure of p-sulfocalix[6]arene, R-, S-BINOL and R-, S-BNA was calculated, and the superamolecular interaction mechanism between analytes and p-sulfocalix[6]arene was disscussed.
Keywords/Search Tags:Nonaqueous capillary electrophoresis(NACE), Calixarene, Electrospray ionization mass spectrometry(ESI-MS), Fragmentation patterns, Chiral separation, 1'-bi-2-naphthol(BINOL), 1,1'-binaphthyl-2,2'-diamine(BNA), Superamolecular interaction
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