【作者】 魏为力；

【导师】 夏之宁；

【作者基本信息】 重庆大学 ， 分析化学， 2007， 硕士

【摘要】 配位相互作用是指可以作为路易斯酸的金属离子与含有孤电子对的路易斯碱以共享电子对的方式发生的相互作用。本论文建立了一种以过渡金属离子为添加剂,以配位相互作用为分离机制的毛细管电泳技术,即配位作用毛细管电泳(CICE)。通过建立CICE技术,在一定程度上扩大了毛细管电泳的分离能力以及分析对象的范围。该CICE技术具有运行介质组成简单、分离选择能力独特、检测灵敏度高以及容易与在线富集技术联用等优点。本论文的主要研究内容如下:①论文第2章对以配位相互作用为分离机制的CICE技术进行了理论上的可行性分析。并对其分离的理论作了公式推导,得出了影响分离的因素,包括运行介质中添加金属离子的种类、浓度以及分析物自身的性质。通过理论分析,得出了对特定分析物所能获得的最佳分离效果。②论文第3章以7种芳香胺类化合物为模型,通过对运行介质酸度、金属离子的种类及浓度、运行电压等因素的考察,建立了CICE技术。并考察了CICE技术对芳香胺类化合物的定量分析能力,验证了其对实际样品进行分析的能力。③论文第4章应用CICE技术对磺胺类药物进行了分析。通过对各分离条件的优化,得到了配位作用毛细管电泳技术分离磺胺类药物的最佳条件为3 mmol/L CuSO4-0.2% CH3COOH(v/v)水溶液作为运行介质,分离电压20 kV。还采用该技术对复方制剂颠茄磺苄啶片中磺胺甲噁唑的含量进行了测定,所得结果与药品的标识量相符合。④论文第5章应用CICE对中药苦参提取物中生物碱类成分进行了分离。配位作用毛细管电泳技术分离苦参提取物的最佳条件为10 mmol/L CuSO4-1 mmol/L柠檬酸水溶液作为运行介质,分离电压15 kV。测定了苦参药材中苦参碱和氧化苦参碱的含量,经配位作用毛细管电泳技术测得苦参碱和氧化苦参碱总含量为2.3%,与中国药典标注量大于1.2%相符。⑤论文第6章利用CICE技术对生物小分子氨基酸进行了分析。优化得到了CICE技术分离氨基酸的最佳条件为:50 mmol/L CuSO4-0.05% CH3COOH(v/v)水溶液作用运行介质,分离电压15 kV。并采用CICE技术实现了绿茶水提物中多种氨基酸的分离。⑥论文第7章提出了一种基于配位相互作用的毛细管电泳在线sweeping富集技术。考察了这种富集技术中,样品进样区带长度对富集效果的影响,结果表明最佳的样品进样区带长度需要综合考虑峰高和半峰宽两个因素。此外,结果还表明这种新型的sweeping技术还具有抗盐富集能力,具有对生物样品进行分析的潜力。最后通过将CICE技术与这种新型sweeping技术联用,对生物样品唾液中的氨基酸实现了分离和检测。本研究建立的CICE技术应用灵活,操作简单并且价格低廉易于推广。更多还原

【Abstract】 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.更多还原