离子色谱/电化学衍生/光学检测联用装置的构建及其应用研究
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摘要
柱后电化学衍生技术目前较多地应用于以反相键合相色谱为主的液相色谱系统中。由于液相色谱使用的流动相具有较窄的pH范围和较高比例的有机试剂含量,液相色谱和电化学衍生技术往往难以兼容。离子色谱使用有机聚合物为基质的固定相,可以使用全pH范围的水溶性缓冲盐作为流动相。这种特征使离子色谱和电化学衍生系统具有较好的兼容性,并且比液相色谱更具优势。本论文在此基础上,设计了两种电化学衍生装置,建立了离子色谱/柱后电化学衍生/光学检测系统来测定极性有机化合物和金属离子,进一步扩大了离子色谱的应用范围。
第一章主要综述了柱后衍生技术包括化学、光化学及电化学衍生法在液相色谱中应用。指出以反相键合相色谱与电化学衍生技术并不具有较好的兼容性,并介绍了离子色谱和以反相键合相色谱在分离方法及使用范围等方面的细微差别,提出了离子色谱-柱后电化学衍生系统的可行性。
第二章设计了一种基于化学镀层平板电极和离子交换膜的电解池,以叶酸和甲氨蝶呤为目标分析物,探讨了该装置的结构、电化学氧化机理、氧化效率及装置性能等问题。并将此电解池作为电化学衍生装置,应用于离子色谱-柱后电化学衍生-荧光分析法中以测定类风湿患者血浆中叶酸和甲氨蝶呤的含量。
第三章以离子色谱-紫外法和离子色谱-柱后电化学衍生-荧光分析法,探讨了以离子色谱分析极性有机物卡马西平的色谱行为,并以此方法测定了癫痫患者血浆中卡马西平的含量,柱后电化学衍生和荧光检测法相结合,使本方法具有较好的灵敏度和选择性。
第四章设计了一种基于多孔电极和离子交换膜的电化学衍生装置,以离子色谱-柱后电化学衍生-荧光法测定了环境水体中的酚类物质。以碱性离子性试剂作为流动相,酚类物质可以再离子色谱分离柱上得到较好的分离效果。由于多孔性电极具有较大的有效电极面积,电化学衍生装置具有较强的氧化能力。在不同的电位下,各种酚类的电化学衍生产物在碱性淋洗液条件下具有较高的灵敏度。离子色谱和电化学衍生、荧光检测的良好兼容性在此工作中得到较好地验证。
第五章以离子色谱-柱后电化学衍生-荧光分析法测定了饮料中的酪氨酸含量。
第六章初步建立了离子色谱-柱后电化学衍生-紫外法测定环境水体中的二价锰离子,在第四章和第五章介绍的基于多孔电极的电化学衍生装置基础上,改变装置结构,初步探讨了装置结构和电化学衍生性能关系。
Post-column electrochemical derivatization (ED) technique is usually used in the reversed phase high performance liquid chromatographic system (RP-HPLC). However, liquid chromatography is not compatible with electrochemical derivatization technique due to the narrow pH range and high proporation of organic solvent used in the mobile phase. The mobile phase of ion chromatography (IC), which is mainly composed of ionized buffer solution, can be used with full pH range since the organic polymer-based ion exchanger is usually employed as stationary phase. This feature lets IC have good compatibility with post-column electrochemical derivatization. The present thesis reported the fabrication of two kinds of electrochemical equipments for derivatization, as well as the method of ion chromatography combined with online post-column electrochemical derivatization and optical detection for the determination of ionized organic species and metal ion, which enlarged the application scope of IC.
There are six parts in the thesis:in the first part, the application of post-column electrochemical derivatization technique used in the liquid chromatographic system was introduced. The poor compatibility between the liquid chromatography and electrochemical derivatization was also pointed out, along with the introduction of slight difference between the RP-HPLC and IC in the fields of separation and application. Finally, the feasibility of ion chromatography combined with electrochemical derivatization was proposed.
In the second part, an electrolytic cell (EC) composed of plannar plated electrode and ion exchange membrane was fabricated. Performances of the cell, such as structure, electro-oxidation mechanism, and electro-oxidation efficiency, were discussed. Using this electrolytic cell, the method of ion chromatography combined with post-column derivatization and fluorescence detection (IC-ED-FD) was developed for the determination of folic acid (FA) and methotraxate (MTX) in the plasma of patients being treated with rheumatoid arthritis (RA) and diffuse large B cell lymphoma.
In the third part, The chromatographic behavior of ionized organic substance (cabarmazepine, CBZ) was studied using IC-UV as well as IC-ED-FD. The determination of CBZ in the plasma of patients of epilepsy was also developed. Good sensitivity and selectivity were obtained due to the combination of electrochemical derivatization and fluorescence detection.
In the fourth part, an electrolytic cell consisting of porous electrode and cation exchange membrane was fabricated. Phenolic compounds were electro-oxidized in this EC after ion chromatographic separation and was then detected fluorometrically. Good separation of phenols was obtained using basic eluent, and the strong electro-oxidation capability of EC could be obtained using porous electrode with large effective surface area. The analysis procedure as well as operation cost was simplified using the basic eluent. Moreover, the sensitivity was improved to a great extent using the porous electrode and time-programmed potential over the EC.
In the fifth part, tyrosine in the baverage was determined using the method described in the fourth part.
Finally, the method of ion chromatography combined with post-column electrochemical derivatization and ultiviolate detection was developed for the determination of magnism (II) in environmental water. The effect between the structure of the EC and electrochemical derivatization performance was prelimilarily discussed.
第一章主要综述了柱后衍生技术包括化学、光化学及电化学衍生法在液相色谱中应用。指出以反相键合相色谱与电化学衍生技术并不具有较好的兼容性,并介绍了离子色谱和以反相键合相色谱在分离方法及使用范围等方面的细微差别,提出了离子色谱-柱后电化学衍生系统的可行性。
第二章设计了一种基于化学镀层平板电极和离子交换膜的电解池,以叶酸和甲氨蝶呤为目标分析物,探讨了该装置的结构、电化学氧化机理、氧化效率及装置性能等问题。并将此电解池作为电化学衍生装置,应用于离子色谱-柱后电化学衍生-荧光分析法中以测定类风湿患者血浆中叶酸和甲氨蝶呤的含量。
第三章以离子色谱-紫外法和离子色谱-柱后电化学衍生-荧光分析法,探讨了以离子色谱分析极性有机物卡马西平的色谱行为,并以此方法测定了癫痫患者血浆中卡马西平的含量,柱后电化学衍生和荧光检测法相结合,使本方法具有较好的灵敏度和选择性。
第四章设计了一种基于多孔电极和离子交换膜的电化学衍生装置,以离子色谱-柱后电化学衍生-荧光法测定了环境水体中的酚类物质。以碱性离子性试剂作为流动相,酚类物质可以再离子色谱分离柱上得到较好的分离效果。由于多孔性电极具有较大的有效电极面积,电化学衍生装置具有较强的氧化能力。在不同的电位下,各种酚类的电化学衍生产物在碱性淋洗液条件下具有较高的灵敏度。离子色谱和电化学衍生、荧光检测的良好兼容性在此工作中得到较好地验证。
第五章以离子色谱-柱后电化学衍生-荧光分析法测定了饮料中的酪氨酸含量。
第六章初步建立了离子色谱-柱后电化学衍生-紫外法测定环境水体中的二价锰离子,在第四章和第五章介绍的基于多孔电极的电化学衍生装置基础上,改变装置结构,初步探讨了装置结构和电化学衍生性能关系。
Post-column electrochemical derivatization (ED) technique is usually used in the reversed phase high performance liquid chromatographic system (RP-HPLC). However, liquid chromatography is not compatible with electrochemical derivatization technique due to the narrow pH range and high proporation of organic solvent used in the mobile phase. The mobile phase of ion chromatography (IC), which is mainly composed of ionized buffer solution, can be used with full pH range since the organic polymer-based ion exchanger is usually employed as stationary phase. This feature lets IC have good compatibility with post-column electrochemical derivatization. The present thesis reported the fabrication of two kinds of electrochemical equipments for derivatization, as well as the method of ion chromatography combined with online post-column electrochemical derivatization and optical detection for the determination of ionized organic species and metal ion, which enlarged the application scope of IC.
There are six parts in the thesis:in the first part, the application of post-column electrochemical derivatization technique used in the liquid chromatographic system was introduced. The poor compatibility between the liquid chromatography and electrochemical derivatization was also pointed out, along with the introduction of slight difference between the RP-HPLC and IC in the fields of separation and application. Finally, the feasibility of ion chromatography combined with electrochemical derivatization was proposed.
In the second part, an electrolytic cell (EC) composed of plannar plated electrode and ion exchange membrane was fabricated. Performances of the cell, such as structure, electro-oxidation mechanism, and electro-oxidation efficiency, were discussed. Using this electrolytic cell, the method of ion chromatography combined with post-column derivatization and fluorescence detection (IC-ED-FD) was developed for the determination of folic acid (FA) and methotraxate (MTX) in the plasma of patients being treated with rheumatoid arthritis (RA) and diffuse large B cell lymphoma.
In the third part, The chromatographic behavior of ionized organic substance (cabarmazepine, CBZ) was studied using IC-UV as well as IC-ED-FD. The determination of CBZ in the plasma of patients of epilepsy was also developed. Good sensitivity and selectivity were obtained due to the combination of electrochemical derivatization and fluorescence detection.
In the fourth part, an electrolytic cell consisting of porous electrode and cation exchange membrane was fabricated. Phenolic compounds were electro-oxidized in this EC after ion chromatographic separation and was then detected fluorometrically. Good separation of phenols was obtained using basic eluent, and the strong electro-oxidation capability of EC could be obtained using porous electrode with large effective surface area. The analysis procedure as well as operation cost was simplified using the basic eluent. Moreover, the sensitivity was improved to a great extent using the porous electrode and time-programmed potential over the EC.
In the fifth part, tyrosine in the baverage was determined using the method described in the fourth part.
Finally, the method of ion chromatography combined with post-column electrochemical derivatization and ultiviolate detection was developed for the determination of magnism (II) in environmental water. The effect between the structure of the EC and electrochemical derivatization performance was prelimilarily discussed.
引文
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