高效液相色譜(HPLC)作為現(xiàn)代分析化學(xué)中最重要的一種分離分析技術(shù),在化學(xué)、生物、醫(yī)藥和環(huán)境科學(xué)等領(lǐng)域得到了廣泛應(yīng)用。近年來,單模式色譜以其高靈敏度、高選擇性和高分離能力等特點(diǎn)得到了快速發(fā)展,但是,在分離復(fù)雜樣品過程中常存在一定的局限性。例如,反相色譜(RPLC)是最常用的色譜模式,對疏水性物質(zhì)具有較強(qiáng)的選擇性和靈敏度,但對強(qiáng)極性和離子型化合物的保留較弱,而且在分離堿性化合物時常導(dǎo)致峰形拖尾、柱效和重復(fù)性變差;離子交換色譜(IEC)常用于分離可解離的或離子型的化合物,但對于帶相同電荷而疏水部分有差異的化合物分離度較差。離子對色譜(IPC)克服了以上困難,通過在流動相中加入離子對試劑,增加了離子型化合物在反相色譜中的保留,能夠同時分離中性和離子型化合物。然而離子對試劑的引入造成柱平衡時間較長,與質(zhì)譜不兼容等缺陷,不適用于梯度洗脫和制備純化,從而限制了IPC在分離分析中的廣泛應(yīng)用。混合模式色譜(MMC)依據(jù)固定相與溶質(zhì)的多種作用機(jī)理,能夠在單一色譜柱上實(shí)現(xiàn)不同的分離模式,而且在混合模式條件下可同時進(jìn)行多種類型樣品的分離檢測。這種無離子對試劑參與的固定相設(shè)計能夠節(jié)約成本、提高工作效率。相比于...

【文章頁數(shù)】：113 頁

【學(xué)位級別】：碩士

【文章目錄】：
摘要
ABSTRACT
Chapter1 Literature Review
    Introduction
    1.1 High Performance Liquid Chromatography
        1.1.1 Principle and Instrument
        1.1.2 Operation Modes
        1.1.3 HPLC Packings
    1.2 Mixed-Mode Chromatography
        1.2.1 RPLC/IEC
        1.2.2 RPLC/HILIC
        1.2.3 HILIC/IEC
        1.2.4 Trimodal Stationary Phase
    1.3 Preparation of Mixed-Mode Stationary Phase
        1.3.1 Chemical Bonding
        1.3.2 Atom Transfer Radical Polymerization
        1.3.3 Click Chemistry
    1.4 Retention Mechanism in Mixed-Mode Chromatography
        1.4.1 Retention Models
        1.4.2 Cooperative Effect
    1.5 Goals and Objectives
Chapter2 Experimental Section
    2.1 Reagents and Instruments
        2.1.1 Reagents
        2.1.2 Materials and Instruments
    2.2.Preparation and Characterization of RP/IEX Stationary Phases
        2.2.1 Preparation of RP/IEX Stationary Phases
        2.2.2 Characterization of RP/SAX Stationary Phases
        2.2.3 Characterization of RP/SCX Stationary Phases
        2.2.4 Application of Mixed-Ligand RP/SCX Stationary Phase
    2.3 Study of Retention Mechanism in Mixed-Mode Chromatography
        2.3.1 Separation of Basic Drugs
        2.3.2 Influence of pH
        2.3.3 Influence of Ionic Strength
        2.3.4 Influence of Solvent Strength
    2.4 Assessing the Contribution of Chelate Cooperativity in Mixed-Mode Chromatography
        2.4.1 Separation of Alkylanilines on RP/SCX Stationary Phases
        2.4.2 Separation of Alkylbenzoic Acids on RP/SAX Stationary Phase
        2.4.3 Separation of Alkylbenzenes on RP/IEX Stationary Phases
Chapter3 Preparation and Characterization of RP/IEX Stationary Phases
    Introduction
    3.1 Preparation and Characterization of RP/SAX Stationary Phases
        3.1.1 Elemental Analysis
        3.1.2 Chromatographic Evaluation
    3.2 Preparation and Characterization of RP/SCX Stationary Phases
        3.2.1 Solid-State¹³C NMR
        3.2.2 Elemental Analysis
        3.2.3 Chromatographic Evaluation
    3.3 Application
        3.3.1 Separation of Melbine and Impurities
        3.3.2 Simultaneous Separation of Acidic,Neutral and Basic Drugs
    3.4 Summary
Chapter4 Study of Retention Mechanisms in Mixed-Mode Chromatography
    Introduction
    4.1 Separation of Basic Drugs on RP/SCX Stationary Phases
    4.2 Influence of pH
    4.3 Influence of Ionic Strength
        4.3.1 Analysis of Retention Mechanism Models
        4.3.2 Quantitative Evaluation of Individual Interactions
        4.3.3 Relationship Between Intercept and Slope for k_T-1/C Plots
    4.4 Influence of Solvent Strength
    4.5 Summary
Chapter5 Assessing the Contribution of Chelate Cooperativity in Mixed-Mode Chromatography
    Introduction
    5.1 Theoretical Model
    5.2 Determination of the Reversed-Phase Retention
    5.3 Determination of the Ion-Exchange Retention
    5.4 Determination of Chelate Cooperativity
    5.5 Relationship Between Intercept and Slope for k_T-1/C Plots
    5.6 Summary
Chapter6 Conclusions and Outlooks
    6.1 Conclusions
    6.2 Outlooks
References
Notes on Publications and Participation in Scientific Research
Acknowledgements



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