论文中文题名: | 复杂基质中杂核NMR技术的分析方法研究与应用 |
姓名: | |
学号: | 20213103021 |
保密级别: | 保密(2年后开放) |
论文语种: | chi |
学科代码: | 0703 |
学科名称: | 理学 - 化学 |
学生类型: | 硕士 |
学位级别: | 理学硕士 |
学位年度: | 2023 |
培养单位: | 西安科技大学 |
院系: | |
专业: | |
研究方向: | 仪器分析化学 |
第一导师姓名: | |
第一导师单位: | |
论文提交日期: | 2023-06-27 |
论文答辩日期: | 2023-06-17 |
论文外文题名: | Research and application of analytical methods of heteronuclear NMR technology in the complex matrix |
论文中文关键词: | |
论文外文关键词: | Methodological study ; NMR ; HMBC ; Boron-containing drugs ; Nitrogen-rich tar ; quantitative analysis |
论文中文摘要: |
复杂基质作为一种化学领域常见分析对象,其分析常常伴随着样品的分离与富集等繁杂的前期处理。核磁共振波谱技术是一种以对样品无损著称的成分结构分析工具,具有样品处理简单,分析快速等优点,但核磁技术在复杂基质中的应用常常会发生严重的信号重叠现象,增加分析难度。本文从杂核NMR技术出发,探究了15N与11B相关NMR技术的分析方法研究与应用,旨在对复杂样品中相关化合物进行针对性的分析。 15N NMR相关技术主要围绕1H-15N HMBC进行探究,选用了2-氟吡啶作为定量NMR检测分析的一种内标物。结果表明,2-氟吡啶在多项NMR实验组中均可实现一定实验浓度范围内的良好线性范围。同时对7种喹啉类标准化合物建立了1H-15N HMBC内标法定量实验,并应用于复杂基质煤焦油,辅以GC-MS对定量方法进行验证,结果发现,两种分析方法对煤焦油样品中喹啉类物质的含量分析结果大致相同。因此2-氟吡啶可看作一种多功能杂核NMR内标物,在多项实验序列中均可建立相关分析方法。这种方法可以在各杂核NMR定量实验中实现桥梁作用,有助于一定程度上消除不同脉冲序列间的各项误差。此方法的建立可用于复杂基质中对含氮杂核结构进行定量分析,为各类含氮复杂样品提供了一种稳健、快捷的分析手段,可以很大程度上弥补现有分析手段在煤焦油样品应用中的不足,对煤焦油组分分析有着重要意义。 11B NMR相关技术主要围绕一维核磁共振技术对常见的含硼中药制剂类的复杂基质中硼的元素形态进行了探究。同时发现属于硼砂的化学位移随着样品浓度的提高会在11B NMR光谱中向高场移动,在无水硼砂D2O样品的11B NMR谱中,11B的化学位移为13 ppm。对1H-11B HMBC的二维核磁共振实验方法进行了初步探究,应用于硼烷-三甲胺络合物并成功检出了相关信号。11B NMR分析方法的建立不仅具有操作简便、不破坏样品等显著优点,而且为中药制剂中有效含硼成分的测定提供了一种新的检测手段,能够对含硼中药制剂的进一步开发做出一定贡献 |
论文外文摘要: |
Complex matrices, as a common analytical object in the field of chemistry, are often accompanied by complex pre-treatments such as sample separation and enrichment. Nuclear magnetic resonance spectroscopy (NMR) technology is a component structure analysis tool known for its non-destructive properties in samples. It has the advantages of simple sample processing and fast analysis. However, the application of NMR technology in complex matrices often results in serious signal overlap, increasing the difficulty of analysis. This article explores the analytical methods and applications of 15N and 11B related NMR techniques based on heteronuclear NMR technology, aiming to conduct targeted analysis of related compounds in complex samples. The 15N NMR-related technology is mainly explored around 1H-15N HMBC, and 2-fluoropyridine was selected as an internal standard for quantitative NMR detection and analysis. The results indicate that 2-fluoropyridine can achieve a good linear range within a certain experimental concentration range in multiple NMR experimental groups. At the same time, 1H-15N HMBC internal standard method quantitative experiment was established for seven quinoline standard compounds and was applied to complex matrix Coal tar. The quantitative method was verified by GC-MS. It was found that the content analysis results of quinoline substances in Coal tar samples by the two analysis methods were roughly the same. Therefore, 2-fluoropyridine can be regarded as a multifunctional heteronuclear NMR internal standard, and correlation analysis methods can be established in multiple experimental sequences. This method can achieve a bridging effect in various heteronuclear NMR quantitative experiments, which helps to eliminate various errors between different pulse sequences to a certain extent. The establishment of this method can be used for quantitative analysis of nitrogen-containing heteronuclear structures in complex matrices, providing a robust and fast analytical method for all kinds of nitrogen-containing complex samples, which can largely make up for the shortcomings of existing analytical methods in the application of Coal tar samples, and is of great significance for the analysis of Coal tar components. The 11B NMR-related technology mainly explores the elemental forms of boron in complex matrices of common boron-containing traditional Chinese medicine preparations using one-dimensional nuclear magnetic resonance technology. At the same time, it is found that the Chemical shift of borax will shift to the high field in the 11B NMR spectrum with the increase of sample concentration. In the 11B NMR spectrum of the anhydrous borax D2O sample, the Chemical shift of 11B is 13 ppm. The two-dimensional nuclear magnetic resonance experiment method of 1H-11B HMBC was preliminarily explored and applied to the borane Trimethylamine complex and successfully detected the relevant signals. The establishment of the 11B NMR analysis method not only has significant advantages such as simple operation and no sample damage but also provides a new detection method for the determination of effective boron-containing components in traditional Chinese medicine preparations, which can make a certain contribution to the further development of boron-containing traditional Chinese medicine preparations. |
中图分类号: | O657.61 |
开放日期: | 2025-06-27 |