核磁共振定量法在化学对照品标化中的应用

目的：建立核磁共振定量法测定多个化学对照品的含量，并与质量平衡法等其他手段含量测定结果进行对比与分析。方法：采用核磁共振技术建立绝对含量测定方法对多个化学对照品的候选原料进行了定性定量检测。结果：本研究通过对测定的结果进行分析，总结核磁定量法解决的问题主要有2类：对于无法溯源的首批对照品的赋值，起到了对质量平衡法结果的佐证作用，并通过对核磁谱图的定性分析，找到核磁定量法、质量平衡法与HPLC外标法等其他含量测定方法结果不匹配的原因；对于含多组分对照品，利用核磁技术可同时对多组分定性定量的优势，可分别测定对照品原料中残留溶剂、盐基和异构体等含量，弥补了一些色谱等方法的不足之处。结论：核磁共振定量方法操作简便，灵敏度高，为对照品辅助定值增加新的重要常用手段。

Objective:To establish the quantity nuclear magnetic method (qNMR) to determine the contents of the reference standard, also compared with mass balance and other methods. Methods:Proton nuclear magnetic resonance spectroscopy (¹H-NMR) spectra were obtained to test and quantity several chemical reference substances (RS) candidate materials by using a Bruker Ascend 500 spectrometer.Result:According to the results, there are two main types of problems can be solved by NMR quantitative analysis:for the first batch of reference materials, it is a supporting assignment way to the mass balance method, sometimes it can found the reason that the results of qNMR method, mass balance method and HPLC external standard method does not match each other;For reference substances containing multi-component, with the advantages of simultaneous qualitative and quantitative determination of multi-component by NMR, the qNMR method can determine the contents of residual solvents, salts and isomers separately, which made up for some shortcomings of chromatographic methods. Conclusion:qNMR provides a simple, rapid and important method for purity analysis of the reference substances.

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