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Development And Application A Capillary Electrophoretic Technique Based On Coordination Interactions

Posted on:2008-06-04Degree:MasterType:Thesis
Country:ChinaCandidate:W L WeiFull Text:PDF
GTID:2121360215990873Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
Most transition metal ions are Lewis acids which can accept lone pair electrons from electron-donating ligands. And this process is called coordination interaction of center ions, mostly transition ions, and ligands. A novel capillary electrophoretic technique based on coordination interaction has been developed. We have defined this technique as coordination interaction capillary electrophoresis (CICE). With the development of CICE, the separation ability and analysis area of capillary electrophoresis are all improved in certain extent. The CICE technique has several advantages such as simple composition of running medium, particular separation selectivity, higher detection sensitivity and easy combination with online preconcentration methods. The research of this thesis mainly includes following parts:①In chapter 2, the possibility of CICE technique was discussed in theory. The separation mechanism was deduced with formulas and the effect factors of separation were proposed such as metal ion nature, concentration, and the properties of the analytes. With theoretical analysis, it can be predicted that how much degree the best separation result can be obtained.②In chapter 3, the CICE technique was developed by utilizing 7 arylamides as model compounds, in which Cu2+ was chosen as additive of the running medium. The limits of detection and linear range of concentration were given for each model compound under the optimum separation conditions. The qualitative and quantitative reliability of the method, as given by resolutions and detection limits, was presented. And the analysis results of degenerative o-penylenediamine sample were obtained and satisfactory.③In chapter 4, sulfonamides were analyzed with CICE technique. The optimum separation conditions for sulfonamides were: 3 mmol/L CuSO4-0.2% CH3COOH (v/v)-H2O and with a 20 kV separation voltage. The content of sulfamethoxazole in Compound Belladonna Sulfamethoxazole and Trimerhoprim Tablets was determined with CICE, and the result was accord with the label amount.④In chapter 5, the alkaloids in the extract of Lightyellow Sophora Root were analyzed by CICE. The optimum separation conditions for the extract of Lightyellow Sophora Root were: 10 mmol/L CuSO4-1 mmol/L citric acid-H2O and with a 15 kV separation voltage. The contents of matrine and oxylmatrine in Lightyellow Sophora Root were determined respectively. The total content of the two alkaloids was determined at 2.3% level and which was coincided with Chinese Pharmacopeia.⑤In chapter 6, the biological micro molecules, amino acids, were analyzed with CICE. The best separation conditions for the amino acids were: 50 mmol/L CuSO4-0.05% CH3COOH (v/v)-H2O as running medium and with a 15 kV separation voltage. The amino acids in a kind of Chinese green tea were successfully separated by CICE what indicated the potential ability of real sample analysis of CICE technique.⑥In chapter 7, a novel sweeping technique was proposed which was based on coordination interactions and thus it was defined as coordination-sweeping. The effect of sample injection zone length on the preconcentrition result was investigated. As the results indicated, the optimum sample injection zone length should be determined with the consideration of both peak height and half peak width. And the salt resist ability of the coordination-sweeping technique was founded. This means that the technique can be applied to the analysis of biological samples. The trace content of amino acids in human saliva were separated and detected by CICE combined with coordination-sweeping technique.In short, the CICE technique developed in this work is simple and flexibility to operate with, and inexpensive to be popularized.
Keywords/Search Tags:Coordination Interaction Capillary Electrophoresis, Arylamides, Aulfonamides, Lightyellow Sophora Root, Amino Acids, Sweeping
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