环境友好型无溶剂法制备键合硅胶色谱固定相
发布时间：2021-01-29 17:46
近年来,随着药物研发技术的快速发展,为人类健康提供了更有利的保障。在药物研发过程中,药物分析发挥着至关重要的作用,它不仅关系到药品的质量控制和质量保证,而且也指导用药安全。由于高效液相色谱法（HPLC）具有高分辨率、高灵敏度、高选择性、与质谱兼容性好等特点,被广泛应用于药物的分离分析和含量测定等研究中。根据中国药典的记载,从1985年到2015年,高效液相色谱法的使用频率由8次增加到3556次,成为药物分析中一种重要的分析方法。高效液相色谱法包括反相液相色谱法（RPLC）、正相液相色谱法（NPLC）、亲水相互作用色谱（HILIC）、离子交换色谱（IEC）以及多模态液相色谱（MMC）。其中,RPLC具有分离效率高、重现性好以及与质谱兼容的特点,是应用最广泛的分离技术,但其只适用于分离非极性或弱极性物质。NPLC能够分离极性物质,但其通常使用非极性或弱极性有机溶剂作为流动相,不适用于在有机溶剂中溶解性差的极性物质,而且流动相中微量的水相就会致使平衡困难或不可逆吸附。HILIC也是一种正相色谱,其流动相可有水相的参与,适用于分离极性物质和亲水性物质,但其对非极性物质的保留很弱。IEC可用于分...
【文章来源】：天津大学天津市 211工程院校 985工程院校 教育部直属院校
【文章页数】：113 页
【学位级别】：硕士
【文章目录】：
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
【参考文献】：
期刊论文
[1]Fe3O4@HKUST-1-C18的制备及用于环境水样中多环芳烃的分析[J]. 陈祥明,张聪,王丹红,李捷,钱疆,谢白璐,石祥程. 分析试验室. 2017(02)
[2]多晶硅流化床反应器内气固两相流场与气泡尺寸分布的TFM-KTGF模拟[J]. 陆时杰,陈彩霞,夏梓洪,倪昊尹. 华东理工大学学报(自然科学版). 2015(06)
[3]混合色谱填料的研究进展[J]. 徐基伟,孙元社,唐涛,夏明珠,雷武,王风云,李彤. 色谱. 2015(11)
[4]万古霉素键合固定相的分离性能[J]. 黄兰淇,周魏华,陈义旺,张凌怡,万益群,张维冰. 色谱. 2013(09)
[5]药物分析研究进展[J]. 李晓冰,石富国,宋沁馨,丁雯,龚楚婷,钱亚芳,丁黎. 药学进展. 2013(08)
[6]巯基-烯/炔点击化学研究进展[J]. 刘清,张秋禹,陈少杰,周健,雷星锋. 有机化学. 2012(10)
[7]巯基-烯点击化学[J]. 徐源鸿,熊兴泉,蔡雷,唐忠科,叶章基. 化学进展. 2012(Z1)
[8]硅胶基质高效液相色谱填料研究进展[J]. 赵贝贝,张艳,唐涛,王风云,张维冰,李彤. 化学进展. 2012(01)
[9]全多孔球形硅胶基质高效液相色谱填料研究进展[J]. 蒋生祥,刘霞. 中国科学（B辑:化学）. 2009(08)
[10]仪器分析方法与分析仪器主要特点及发展现状综述[J]. 孙英鸿,齐懿鸣,王琛琛,杨玉霞. 生命科学仪器. 2009(01)
本文编号：3007313
【文章来源】：天津大学天津市 211工程院校 985工程院校 教育部直属院校
【文章页数】：113 页
【学位级别】：硕士
【文章目录】：
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
【参考文献】：
期刊论文
[1]Fe3O4@HKUST-1-C18的制备及用于环境水样中多环芳烃的分析[J]. 陈祥明,张聪,王丹红,李捷,钱疆,谢白璐,石祥程. 分析试验室. 2017(02)
[2]多晶硅流化床反应器内气固两相流场与气泡尺寸分布的TFM-KTGF模拟[J]. 陆时杰,陈彩霞,夏梓洪,倪昊尹. 华东理工大学学报(自然科学版). 2015(06)
[3]混合色谱填料的研究进展[J]. 徐基伟,孙元社,唐涛,夏明珠,雷武,王风云,李彤. 色谱. 2015(11)
[4]万古霉素键合固定相的分离性能[J]. 黄兰淇,周魏华,陈义旺,张凌怡,万益群,张维冰. 色谱. 2013(09)
[5]药物分析研究进展[J]. 李晓冰,石富国,宋沁馨,丁雯,龚楚婷,钱亚芳,丁黎. 药学进展. 2013(08)
[6]巯基-烯/炔点击化学研究进展[J]. 刘清,张秋禹,陈少杰,周健,雷星锋. 有机化学. 2012(10)
[7]巯基-烯点击化学[J]. 徐源鸿,熊兴泉,蔡雷,唐忠科,叶章基. 化学进展. 2012(Z1)
[8]硅胶基质高效液相色谱填料研究进展[J]. 赵贝贝,张艳,唐涛,王风云,张维冰,李彤. 化学进展. 2012(01)
[9]全多孔球形硅胶基质高效液相色谱填料研究进展[J]. 蒋生祥,刘霞. 中国科学（B辑:化学）. 2009(08)
[10]仪器分析方法与分析仪器主要特点及发展现状综述[J]. 孙英鸿,齐懿鸣,王琛琛,杨玉霞. 生命科学仪器. 2009(01)
本文编号：3007313
本文链接：https://www.wllwen.com/kejilunwen/huaxue/3007313.html
教材专著
