近年來,隨著藥物研發(fā)技術(shù)的快速發(fā)展,為人類健康提供了更有利的保障。在藥物研發(fā)過程中,藥物分析發(fā)揮著至關(guān)重要的作用,它不僅關(guān)系到藥品的質(zhì)量控制和質(zhì)量保證,而且也指導(dǎo)用藥安全。由于高效液相色譜法（HPLC）具有高分辨率、高靈敏度、高選擇性、與質(zhì)譜兼容性好等特點,被廣泛應(yīng)用于藥物的分離分析和含量測定等研究中。根據(jù)中國藥典的記載,從1985年到2015年,高效液相色譜法的使用頻率由8次增加到3556次,成為藥物分析中一種重要的分析方法。高效液相色譜法包括反相液相色譜法（RPLC）、正相液相色譜法（NPLC）、親水相互作用色譜（HILIC）、離子交換色譜（IEC）以及多模態(tài)液相色譜（MMC）。其中,RPLC具有分離效率高、重現(xiàn)性好以及與質(zhì)譜兼容的特點,是應(yīng)用最廣泛的分離技術(shù),但其只適用于分離非極性或弱極性物質(zhì)。NPLC能夠分離極性物質(zhì),但其通常使用非極性或弱極性有機溶劑作為流動相,不適用于在有機溶劑中溶解性差的極性物質(zhì),而且流動相中微量的水相就會致使平衡困難或不可逆吸附。HILIC也是一種正相色譜,其流動相可有水相的參與,適用于分離極性物質(zhì)和親水性物質(zhì),但其對非極性物質(zhì)的保留很弱。IEC可用于分... 

【文章來源】：天津大學(xué)天津市 211工程院校 985工程院校 教育部直屬院校

【文章頁數(shù)】：113 頁

【學(xué)位級別】：碩士

【文章目錄】：
摘要
ABSTRACT
Chapter1 Literature reviews
    Introduction
    1.1 Drug analysis in drug development
        1.1.1 Process of drug research
        1.1.2 Methods of drug analysis
    1.2 High performance liquid chromatography
        1.2.1 Reversed phase liquid chromatography
        1.2.2 Normal phase liquid chromatography
        1.2.3 Hydrophilic interaction liquid chromatography
        1.2.4 Ion exchange liquid chromatography
        1.2.5 Molecular exclusion chromatography
        1.2.6 Mixed-mode liquid chromatography
    1.3 Supports of HPLC packings
        1.3.1 Inorganic supports
        1.3.2 Organic supports
        1.3.3 Organic-inorganic hybrid supports
    1.4 Preparation of chemically bonded silica stationary phase
        1.4.1 Organic solvent methods
        1.4.2 Supercritical fluid methods
        1.4.3 Fluidised-bed reactor methods
        1.4.4 Vapor deposition methods
        1.4.5 Click chemistry
    1.5 Characterization and evaluation
        1.5.1 Nitrogen adsorption isotherm
        1.5.2 Infrared spectroscopy
        1.5.3 Nuclear magnetic resonance technique
        1.5.4 Elemental analysis
        1.5.5 Chromatographic evaluation
    1.6 Retention mechanism
        1.6.1 Linear solvation energy relationships
        1.6.2 Multiple sites model
    1.7 Objectives
Chapter2 Experimental
    2.1 Materials and instruments
        2.1.1 Materials
        2.1.2 Instruments
18 reversed-phase packing">    2.2 Preparation and characterization of C₁₈ reversed-phase packing
        2.2.1 Preparation
        2.2.2 Optimization of preparation conditions
18 reversed phase by different methods">        2.2.3 Preparation of C₁₈ reversed phase by different methods
        2.2.4 Characterization
        2.2.5 Evaluation and chromatographic conditions
    2.3 Preparation and characterization of thioether-embedded cyano stationary phase
        2.3.1 Preparation
        2.3.2 Characterization
        2.3.3 Chromatographic evaluation
        2.3.4 Hydrolytic stability
        2.3.5 Chromatographic conditions
    2.4 Retention mechanisms on thioether-embedded cyano stationary phase
        2.4.1 Tanaka tests
        2.4.2 Linear solvation energy relationships
        2.4.3 Multiple sites model
18 reversed-phase packing">Chapter3 Preparation of C₁₈ reversed-phase packing
    Introduction
    3.1 Optimized conditions
        3.1.1 Effect of impregnation solvents
        3.1.2 Effect of impregnation time
        3.1.3 Effect of octadecyl silane amount
        3.1.4 Effect of octadecyl silane types
18 reversed phase">    3.2 Preparation of C₁₈ reversed phase
        3.2.1 Synthesis and characterization
        3.2.2 Chromatographic evaluation
        3.2.3 Reproducibility
    3.3 Conclusions
Chapter4 Preparation of thiol-embedded cyano packing
    Introduction
    4.1 Synthesis and characterization
    4.2 Chromatographic evaluation
        4.2.1 Retention characteristics under RPLC mode
        4.2.2 Retention characteristics under HILIC mode
        4.2.3 Retention characteristics under RPLC/HILIC mode
    4.3 Accelerated stability test
    4.4 Conclusions
Chapter5 Retention mechanism of thiol-embedded cyano bonded packing
    Introduction
    5.1 Tanaka tests
    5.2 Linear solvation energy relationships
    5.3 Multiple sites model
        5.3.1 Effect of eluent pH on retention
        5.3.2 Effect of ionic strength on retention
        5.3.3 Effect of solvent strength on retention
    5.4 Conclusions
Chapter6 Conclusions and outlooks
    6.1 Conclusions
    6.2 Outlooks
References
Notes on publications and participation in scientific research
Acknowledgements


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