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氟磷谱定量核磁共振法进展综述

黄挺 吴华鑫

黄挺,吴华鑫. 氟磷谱定量核磁共振法进展综述[J]. 计量科学与技术,2023, 67(5): 9-15 doi: 10.12338/j.issn.2096-9015.2023.0095
引用本文: 黄挺,吴华鑫. 氟磷谱定量核磁共振法进展综述[J]. 计量科学与技术,2023, 67(5): 9-15 doi: 10.12338/j.issn.2096-9015.2023.0095
HUANG Ting, WU Huaxin. A Review on the Advancements in Quantitative Nuclear Magnetic Resonance Spectroscopy of Fluorine and Phosphorus[J]. Metrology Science and Technology, 2023, 67(5): 9-15. doi: 10.12338/j.issn.2096-9015.2023.0095
Citation: HUANG Ting, WU Huaxin. A Review on the Advancements in Quantitative Nuclear Magnetic Resonance Spectroscopy of Fluorine and Phosphorus[J]. Metrology Science and Technology, 2023, 67(5): 9-15. doi: 10.12338/j.issn.2096-9015.2023.0095

氟磷谱定量核磁共振法进展综述

doi: 10.12338/j.issn.2096-9015.2023.0095
基金项目: 中国计量科学研究院基本科研业务费项目(21-AKYZZ2120-21)。
详细信息
    作者简介:

    黄挺(1979-),中国计量科学研究院研究员,研究方向:化学计量、分析化学等,邮箱:huangting@nim.ac.cn

  • 中图分类号: TB99

A Review on the Advancements in Quantitative Nuclear Magnetic Resonance Spectroscopy of Fluorine and Phosphorus

  • 摘要: 定量核磁共振法(qNMR)作为一种选择性强、准确快捷的定量分析方法,广泛应用于有机化合物的纯度定值。它作为潜在基准方法,在国际计量比对中得到越来越广泛的关注与应用,而且最新的国际计量发展规划计划将其从传统的氢谱(1H)扩展至氟谱、磷谱的技术领域。随着qNMR在代谢组学、环境分析和生理学研究等新的领域的应用,引入了天然产物、生物分子、蛋白质和代谢物等更复杂的分子和系统,使得常用的1H-qNMR遇到很大挑战,因此基于氟(19F)和磷(31P)等具有核磁共振特性核的qNMR日益受到重视。与1H-qNMR相比,氟谱和磷谱具有相近的灵敏度、更高的分辨能力,可以排除残留溶剂或水峰的干扰。介绍了19F-qNMR和31P-qNMR的特性优势、方法上的改进性和近年来在各领域的研究进展。在19F-qNMR和31P-qNMR方法学研究中,重点在具有溯源性的标准物质的研制、同轴插入内标方法、参数优化等方面。在应用领域,19F-qNMR重点集中于医药、材料、环境等领域,31P-qNMR集中于食品、医药、生物等领域。
  • 表  1  19F-qNMR与类似技术的比较

    Table  1.   Comparison of 19F-qNMR with analogous techniques

    类似技术 项目 19F-qNMR结果 类似技术结果 文献
    1H- qNMR 线性 0.9999 0.9999 [18]
    精度 0.49% 0.82% [18]
    重复性 0.73% 0.62% [18]
    定量限(mg/mL) 1.34 1.02 [18]
    平均值 93.1% 95.3% [18]
    RSD 0.73% 0.62% [18]
    回收率 98.7% 98.6% [18]
    滴定性 当量重量(g/eq) 385 393 [23]
    气相色谱-
    质谱法
    雨水中的三
    氟乙酸(ng/L)
    80 83 [33]
    185 200 [33]
    850 810 [33]
    下载: 导出CSV

    表  2  31P-qNMR与类似技术的比较

    Table  2.   Comparison of 31P-qNMR with analogous techniques

    类似技术 项目 31P-qNMR
    结果
    类似技
    术结果
    文献
    液相色谱 磷霉素钙(mg/tablet) 511 516 [36]
    杂质A含量 2.12% 2.05% [36]
    离子交换色谱 焦磷酸钠 96.01% 96.32% [39]
    1H- qNMR TPPTS 58.51% 58.72 [45]
    二维薄层色谱 磷脂酰胆碱 25.3% 25.4% [47]
    磷脂酰乙醇胺 25.4% 21.8% [47]
    磷脂酰肌醇 13.6% 14.0% [47]
    离子色谱法 PO43− (g/kg) 3.50 3.34 [49]
    P2O74− (g/kg) 0.61 0.59 [49]
    1H- qNMR 索非布韦 99.44% 99.10% [50]
    下载: 导出CSV
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出版历程
  • 收稿日期:  2023-03-30
  • 录用日期:  2023-04-23
  • 修回日期:  2023-05-19
  • 网络出版日期:  2023-07-06
  • 刊出日期:  2023-05-31

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