【作者】 李晶；

【导师】 朱岩；

【作者基本信息】 浙江大学 ， 分析化学， 2009， 博士

【摘要】 近几年来,随着科技进步,离子色谱已经从简单的离子测定向着快速分离分析、新型高效色谱固定相开发以及仪器微型化等领域深入发展。整体型色谱固定相作为一种新型的分离介质,具有制备过程简单、易于改性、通透性能好、柱压低和独特的传质方式等优点,已经成为离子色谱发展中的热点。本文利用表面活性剂改性硅胶基质整体柱,得到具有离子交换功能的色谱固定相,研究了涂覆机理,考察了改性柱的稳定性,优化了色谱分离条件,结合整体柱良好的传质性能,应用于生物医药样品的快速分离和检测。以聚甲基丙烯酸缩水甘油酯整体柱为基质,通过原位聚合的方法,分别制备了常规型和毛细管型的色谱柱,利用三甲胺修饰改性成为具有阴离子交换功能的固定相,研究了聚合和改性条件对柱交换容量的影响,优化分离条件,应用于商品化离子色谱系统和自建的毛细管离子色谱系统中,分离检测常见无机阴离子；利用亚硫酸钠修饰改性带有环氧功能基的聚合物基质,制备具有阳离子交换功能基团的毛细管离子交换色谱柱,采用流速梯度淋洗方式应用于常见无机阳离子的分离检测,并在该色谱柱的基础上利用季铵型乳胶修饰改性制备成了乳胶涂覆型阴离子交换色谱柱,应用于常规阴离子的检测中。利用低流速泵、微量进样器以及自制的毛细管离子色谱柱,构建了毛细管离子色谱系统,并结合紫外检测器以及电导检测器,利用直接、间接紫外检测；接触式和非接触式电导检测技术对阴阳离子进行了检测,评价了不同检测器的性能,并应用于阴阳离子分离分析以及实际样品(水样、奶粉样品)的检测。更多还原

【Abstract】 In recent years, ion chromatography (IC) has been further developed in some new research fields:fast & ultra-fast analysis; new stationary phases with higher efficiency and better selectivity; miniaturization of the whole system. For these progresses, the monolithic stationary phases have possessed key position with the special advantages like ease for preparation and modification, low flow resistance and attractive hydrodynamic characteristics, etc.Silica-based monolithic column coated with surfactant was used for pharmaceutical analysis in traditional IC. The process and mechanism of coating with good reproducibility and stability were studied. Due to the low pressure under a higher flow rate, the coated column can be applied for fast separation and determination of anions and ionized compounds in drug samples.Reactive continuous rods of macroporous poly (glycidyl methacrylate-co ethylene dimethacrylate) have been prepared by "in-situ" copolymerization of the monomers in the presence of porogens. Different sizes of anion-exchange monolithic columns (traditional ones 4.6 mm I.D. and capillaries 530 & 320μm I.D.) were obtained by the modification of the matrix with trimethylamine. With the optimized reaction conditions, these columns were used for separation of anions in commercial & capillary IC system; respectively. The GMA-based matrix also can be modified with sodium sulfite for cation-exchange column that can be used in capillary IC for the separation of cations by flow rate gradient elution. Based on the above techniques, quaternary ammonium functionalized latex was applied for the preparation of anion-exchange capillary monolithic column. With the optimized chromatographic conditions, the latex-coated column was used for separation of common anions.A novel capillary IC system was established composed with a LC pump (flow rate lower toμL/min), micro injector with a 500 nL injection volume, a prepared capillary monolithic column and different detectors. With a capillary UV detection cell, anions and cations were determined by direct or indirect UV detection, respectively. Two kinds of conductivity detectors-contact conductivity detector and the contactless one, were introduced into the system for determination of ions. It’s compared and evaluated with different detection ways as well as the whole micro-IC system, which was successfully used for analysis of real samples such as water samples and milk powder samples.更多还原